WorldWideScience

Sample records for ultra-high mass resolving

  1. Molecular composition of organic aerosols in central Amazonia: an ultra-high-resolution mass spectrometry study

    OpenAIRE

    Kourtchev, I; Godoi, RHM; Connors, S; Levine, JG; Archibald, AT; Godoi, AFL; Paralovo, SL; Barbosa, CGG; Souza, RAF; Manzi, AO; Seco, R; Sjostedt, S; Park, J-H; Guenther, A; Kim, S

    2016-01-01

    The Amazon Basin plays key role in atmospheric chemistry, biodiversity and climate change. In this study we applied nanoelectrospray (nanoESI) ultra-high-resolution mass spectrometry (UHRMS) for the analysis of the organic fraction of PM$_{2.5}$ aerosol samples collected during dry and wet seasons at a site in central Amazonia receiving background air masses, biomass burning and urban pollution. Comprehensive mass spectral data evaluation methods (e.g. Kendrick mass defect, Van Krevelen diagr...

  2. Fast and sensitive analysis of beta blockers by ultra-high-performance liquid chromatography coupled with ultra-high-resolution TOF mass spectrometry.

    Science.gov (United States)

    Tomková, Jana; Ondra, Peter; Kocianová, Eva; Václavík, Jan

    2017-07-01

    This paper presents a method for the determination of acebutolol, betaxolol, bisoprolol, metoprolol, nebivolol and sotalol in human serum by liquid-liquid extraction and ultra-high-performance liquid chromatography coupled with ultra-high-resolution TOF mass spectrometry. After liquid-liquid extraction, beta blockers were separated on a reverse-phase analytical column (Acclaim RS 120; 100 × 2.1 mm, 2.2 μm). The total run time was 6 min for each sample. Linearity, limit of detection, limit of quantification, matrix effects, specificity, precision, accuracy, recovery and sample stability were evaluated. The method was successfully applied to the therapeutic drug monitoring of 108 patients with hypertension. This method was also used for determination of beta blockers in 33 intoxicated patients. Copyright © 2016 John Wiley & Sons, Ltd.

  3. Radio reconstruction of the mass of ultra-high cosmic rays

    Energy Technology Data Exchange (ETDEWEB)

    Dorosti, Qader [Institut fuer Kernphysik (IKP), KIT (Germany)

    2015-07-01

    Detection of ultra-high energy cosmic rays can reveal the processes of the most violent sources in the Universe, which yet has to be determined. Interaction of cosmic rays with the Earth's atmosphere results in cascades of secondary particles, i.e. air showers. Many of such particles are electrons and positrons. The induced electrons and positrons interact with the geomagnetic field and induce radio emissions. Detection of air showers along with the detection of induced radio emissions can furnish a precise measurement of the direction, energy and mass of ultra-high energy cosmic rays. The Auger Engineering Radio Array consists of 124 radio stations measuring radio emission from air showers, in order to reconstruct the energy, direction and mass of cosmic rays. In this contribution, we present a method which employs a reduced hyperbolic model to describe the shape of radio wave front. We have investigated that the parameters of the reduced hyperbolic model are sensitive to the mass of cosmic rays. The obtained results are presented in this talk.

  4. Chemical fingerprint of Ganmaoling granule by double-wavelength ultra high performance liquid chromatography and ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Lou, Qiong; Ye, Xiaolan; Zhou, Yingyi; Li, Hua; Song, Fenyun

    2015-06-01

    A method incorporating double-wavelength ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry was developed for the investigation of the chemical fingerprint of Ganmaoling granule. The chromatographic separations were performed on an ACQUITY UPLC HSS C18 column (2.1 × 50 mm, 1.8 μm) at 30°C using gradient elution with water/formic acid (1%) and acetonitrile at a flow rate of 0.4 mL/min. A total of 11 chemical constituents of Ganmaoling granule were identified from their molecular weight, UV spectra, tandem mass spectrometry data, and retention behavior by comparing the results with those of the reference standards or literature. And 25 peaks were selected as the common peaks for fingerprint analysis to evaluate the similarities among 25 batches of Ganmaoling granule. The results of principal component analysis and orthogonal projection to latent structures discriminant analysis showed that the important chemical markers that could distinguish the different batches were revealed as 4,5-di-O-caffeoylquinic acid, 3,5-di-O-caffeoylquinic acid, and 4-O-caffeoylquinic acid. This is the first report of the ultra high performance liquid chromatography chemical fingerprint and component identification of Ganmaoling granule, which could lay a foundation for further studies of Ganmaoling granule. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Low temperature growth of ultra-high mass density carbon nanotube forests on conductive supports

    International Nuclear Information System (INIS)

    Sugime, Hisashi; Esconjauregui, Santiago; Yang, Junwei; D'Arsié, Lorenzo; Robertson, John; Oliver, Rachel A.; Bhardwaj, Sunil; Cepek, Cinzia

    2013-01-01

    We grow ultra-high mass density carbon nanotube forests at 450 °C on Ti-coated Cu supports using Co-Mo co-catalyst. X-ray photoelectron spectroscopy shows Mo strongly interacts with Ti and Co, suppressing both aggregation and lifting off of Co particles and, thus, promoting the root growth mechanism. The forests average a height of 0.38 μm and a mass density of 1.6 g cm −3 . This mass density is the highest reported so far, even at higher temperatures or on insulators. The forests and Cu supports show ohmic conductivity (lowest resistance ∼22 kΩ), suggesting Co-Mo is useful for applications requiring forest growth on conductors

  6. Ultra High-Mass Resolution Paper Spray by Fourier Transform Ion Cyclotron Resonance Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Kevin D. Quinn

    2012-01-01

    Full Text Available Paper Spray Ionization is an atmospheric pressure ionization technique that utilizes an offline electro-osmotic flow to generate ions off a paper medium. This technique can be performed on a Bruker SolariX Fourier transform ion cyclotron resonance mass spectrometer by modifying the existing nanospray source. High-resolution paper spray spectra were obtained for both organic and biological samples to demonstrate the benefit of linking the technique with a high-resolution mass analyzer. Error values in the range 0.23 to 2.14 ppm were obtained for calf lung surfactant extract with broadband mass resolving power (m/Δm50% above 60,000 utilizing an external calibration standard.

  7. Ultra high energy cosmic rays: clustering, GUT scale and neutrino masses

    International Nuclear Information System (INIS)

    Fodor, Z.

    2002-01-01

    The clustering of ultra high energy (above 5 · 10 19 eV) cosmic rays (UHECR) suggests that they might be emitted by compact sources. We present a statistical analysis on the source density based on the multiplicities. The propagation of UHECR protons is studied in detail. The UHECR spectrum is consistent with the decay of GUT scale particles and/or with the Z-burst. The predicted GUT mass is m x = 10 b GeV, where b 14.6 -1.7 +1.6 . Our neutrino mass prediction depends on the origin of the power part of the spectrum: m ν = 2.75 -0.97 +1.28 eV for halo and 0.26 -0.14 +0.20 eV for extragalactic (EG) origin

  8. SIEMENS ADVANCED QUANTRA FTICR MASS SPECTROMETER FOR ULTRA HIGH RESOLUTION AT LOW MASS

    Energy Technology Data Exchange (ETDEWEB)

    Spencer, W; Laura Tovo, L

    2008-07-08

    The Siemens Advanced Quantra Fourier Transform Ion Cyclotron Resonance (FTICR) mass spectrometer was evaluated as an alternative instrument to large double focusing mass spectrometers for gas analysis. High resolution mass spectrometers capable of resolving the common mass isomers of the hydrogen isotopes are used to provide data for accurate loading of reservoirs and to monitor separation of tritium, deuterium, and helium. Conventional double focusing magnetic sector instruments have a resolution that is limited to about 5000. The Siemens FTICR instrument achieves resolution beyond 400,000 and could possibly resolve the tritium ion from the helium-3 ion, which differ by the weight of an electron, 0.00549 amu. Working with Y-12 and LANL, SRNL requested Siemens to modify their commercial Quantra system for low mass analysis. To achieve the required performance, Siemens had to increase the available waveform operating frequency from 5 MHz to 40 MHz and completely redesign the control electronics and software. However, they were able to use the previous ion trap, magnet, passive pump, and piezo-electric pulsed inlet valve design. NNSA invested $1M in this project and acquired four systems, two for Y-12 and one each for SRNL and LANL. Siemens claimed a $10M investment in the Quantra systems. The new Siemens Advanced Quantra demonstrated phenomenal resolution in the low mass range. Resolution greater than 400,000 was achieved for mass 2. The new spectrometer had a useful working mass range to 500 Daltons. However, experiments found that a continuous single scan from low mass to high was not possible. Two useful working ranges were established covering masses 1 to 6 and masses 12 to 500 for our studies. A compromise performance condition enabled masses 1 to 45 to be surveyed. The instrument was found to have a dynamic range of about three orders of magnitude and quantitative analysis is expected to be limited to around 5 percent without using complex fitting algorithms

  9. Development of filter element from nanocomposites of ultra high molar mass polyethylene having silver nanoparticles

    International Nuclear Information System (INIS)

    Bizzo, Maurizio A.; Wang, S. Hui

    2015-01-01

    The production of polymer based filter elements for water is widespread in the market but has an undesirable characteristic, they are not always efficient and capable of retaining or eliminating microorganisms. This paper proposes the production of filters with biocidal activity, comprised by nanocomposites of ultra-high molar mass polyethylene (UHMMPE) containing silver nanoparticles. The polymer is responsible for the uniform porous structure of the filter element and the Ag nanoparticles for its biocidal action. The filter elements were produced from two kinds of UHMMPE particles with different particle size distributions, one in the range of 150 to 200μm and the other of 300 to 400μm. Samples were collected from the obtained filter elements and characterized by X-ray diffractometry, scanning electron microscopy and microanalysis. The results indicated the formation of nanocomposite containing silver nanoparticles. (author)

  10. Next-generation technologies for spatial proteomics: Integrating ultra-high speed MALDI-TOF and high mass resolution MALDI FTICR imaging mass spectrometry for protein analysis.

    Science.gov (United States)

    Spraggins, Jeffrey M; Rizzo, David G; Moore, Jessica L; Noto, Michael J; Skaar, Eric P; Caprioli, Richard M

    2016-06-01

    MALDI imaging mass spectrometry is a powerful analytical tool enabling the visualization of biomolecules in tissue. However, there are unique challenges associated with protein imaging experiments including the need for higher spatial resolution capabilities, improved image acquisition rates, and better molecular specificity. Here we demonstrate the capabilities of ultra-high speed MALDI-TOF and high mass resolution MALDI FTICR IMS platforms as they relate to these challenges. High spatial resolution MALDI-TOF protein images of rat brain tissue and cystic fibrosis lung tissue were acquired at image acquisition rates >25 pixels/s. Structures as small as 50 μm were spatially resolved and proteins associated with host immune response were observed in cystic fibrosis lung tissue. Ultra-high speed MALDI-TOF enables unique applications including megapixel molecular imaging as demonstrated for lipid analysis of cystic fibrosis lung tissue. Additionally, imaging experiments using MALDI FTICR IMS were shown to produce data with high mass accuracy (z 5000) for proteins up to ∼20 kDa. Analysis of clear cell renal cell carcinoma using MALDI FTICR IMS identified specific proteins localized to healthy tissue regions, within the tumor, and also in areas of increased vascularization around the tumor. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Interaction of ultra-high intensity laser pulse with a mass limited targets

    International Nuclear Information System (INIS)

    Andreev, A.A.; Platonov, K.Yu.; Limpouch, J.; Psikal, J.; Kawata, S.

    2006-01-01

    Complete test of publication follows. Ultra-high intensity laser pulses may be produced now via CPA scheme by using very short laser pulses of a relatively low energy. Interaction of such pulses with massive target is not very efficient as the energy delivered to charged particles spreads out quickly over large distances and it is redistributed between many secondary particles. One possibility to limit this undesirable energy spread is to use mass limited targets (MLT), for example droplets, big clusters or small foil sections. This is an intermediate regime in target dimensions between bulk solid and nanometer-size atomic cluster targets. A few experimental and theoretical studies have been carried out on laser absorption, fast particle generation and induced nuclear fusion reactions in the interaction of ultrashort laser pulses with MLT plasma. We investigate here laser interactions with MLT via 2D3V relativistic electromagnetic PIC simulations. We assume spherical droplet as a typical MLT. However, the sphere is represented in 2D simulations by an infinite cylinder irradiated uniformly along its length. We assume that MLT is fully ionized before main pulse interaction either due to insufficient laser contrast or due to a prepulse. For simplicity, we assume homogeneous plasma of high initial temperature. We analyze the interaction of relativistic laser pulses of various polarizations with targets of different shapes, such as a foil, quadrant and sphere. The mechanisms of laser absorption, electron and ion acceleration are clarified for different laser and target parameters. When laser interacts with the target front side, kinetic energy of electrons rises rapidly with fast oscillations in the kinetic and field energy, caused by electron oscillations in the laser field. Small energy oscillations, observed later, are caused by the electron motion back and forth through the droplet. Approximately 40% of laser energy is transferred to the kinetic energy of electrons

  12. Quantitative Analysis of Ingenol in Euphorbia species via Validated Isotope Dilution Ultra-high Performance Liquid Chromatography Tandem Mass Spectrometry

    Czech Academy of Sciences Publication Activity Database

    Béres, T.; Dragull, K.; Pospíšil, Jiří; Tarkowská, Danuše; Dančák, M.; Bíba, Ondřej; Tarkowski, P.; Doležal, K.; Strnad, Miroslav

    2018-01-01

    Roč. 29, č. 1 (2018), s. 23-29 ISSN 0958-0344 R&D Projects: GA ČR GA17-14007S; GA MŠk(CZ) LO1204 Institutional support: RVO:61389030 Keywords : Euphorbia genus * ingenol * isotope-dilution method * mass spectrometry * ultra-high performance liquid chromatography Subject RIV: FD - Oncology ; Hematology OBOR OECD: Analytical chemistry Impact factor: 2.292, year: 2016

  13. Rapid screening for drugs of abuse in biological fluids by ultra high performance liquid chromatography/Orbitrap mass spectrometry.

    Science.gov (United States)

    Jagerdeo, Eshwar; Schaff, Jason E

    2016-08-01

    We present a UPLC(®)-High Resolution Mass Spectrometric method to simultaneously screen for nineteen benzodiazepines, twelve opiates, cocaine and three metabolites, and three "Z-drug" hypnotic sedatives in both blood and urine specimens. Sample processing consists of a high-speed, high-temperature enzymatic hydrolysis for urine samples followed by a rapid supported liquid extraction (SLE). The combination of ultra-high resolution chromatography with high resolution mass spectrometry allows all 38 analytes to be uniquely detected with a ten minute analytical run. Limits of detection for all target analytes are 3ng/mL or better, with only 0.3mL of specimen used for analysis. The combination of low sample volume with fast processing and analysis makes this method a suitable replacement for immunoassay screening of the targeted drug classes, while providing far superior specificity and better limits of detection than can routinely be obtained by immunoassay. Published by Elsevier B.V.

  14. [Qualitative and quantitative analysis of amygdalin and its metabolite prunasin in plasma by ultra-high performance liquid chromatography-tandem quadrupole time of flight mass spectrometry and ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry].

    Science.gov (United States)

    Gao, Meng; Wang, Yuesheng; Wei, Huizhen; Ouyang, Hui; He, Mingzhen; Zeng, Lianqing; Shen, Fengyun; Guo, Qiang; Rao, Yi

    2014-06-01

    A method was developed for the determination of amygdalin and its metabolite prunasin in rat plasma after intragastric administration of Maxing shigan decoction. The analytes were identified by ultra-high performance liquid chromatography-tandem quadrupole time of flight mass spectrometry and quantitatively determined by ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry. After purified by liquid-liquid extraction, the qualitative analysis of amygdalin and prunasin in the plasma sample was performed on a Shim-pack XR-ODS III HPLC column (75 mm x 2.0 mm, 1.6 microm), using acetonitrile-0.1% (v/v) formic acid aqueous solution. The detection was performed on a Triple TOF 5600 quadrupole time of flight mass spectrometer. The quantitative analysis of amygdalin and prunasin in the plasma sample was performed by separation on an Agilent C18 HPLC column (50 mm x 2.1 mm, 1.7 microm), using acetonitrile-0.1% (v/v) formic acid aqueous solution. The detection was performed on an AB Q-TRAP 4500 triple quadrupole mass spectrometer utilizing electrospray ionization (ESI) interface operated in negative ion mode and multiple-reaction monitoring (MRM) mode. The qualitative analysis results showed that amygdalin and its metabolite prunasin were detected in the plasma sample. The quantitative analysis results showed that the linear range of amygdalin was 1.05-4 200 ng/mL with the correlation coefficient of 0.999 0 and the linear range of prunasin was 1.25-2 490 ng/mL with the correlation coefficient of 0.997 0. The method had a good precision with the relative standard deviations (RSDs) lower than 9.20% and the overall recoveries varied from 82.33% to 95.25%. The limits of detection (LODs) of amygdalin and prunasin were 0.50 ng/mL. With good reproducibility, the method is simple, fast and effective for the qualitative and quantitative analysis of the amygdalin and prunasin in plasma sample of rats which were administered by Maxing shigan decoction.

  15. New approach to the determination phosphorothioate oligonucleotides by ultra high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Studzińska, Sylwia; Mounicou, Sandra; Szpunar, Joanna; Łobiński, Ryszard; Buszewski, Bogusław

    2015-01-15

    This text presents a novel method for the separation and detection of phosphorothioate oligonucleotides with the use of ion pair ultra high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry The research showed that hexafluoroisopropanol/triethylamine based mobile phases may be successfully used when liquid chromatography is coupled with such elemental detection. However, the concentration of both HFIP and TEA influences the final result. The lower concentration of HFIP, the lower the background in ICP-MS and the greater the sensitivity. The method applied for the analysis of serum samples was based on high resolution inductively coupled plasma mass spectrometry. Utilization of this method allows determination of fifty times lower quantity of phosphorothioate oligonucleotides than in the case of quadrupole mass analyzer. Monitoring of (31)P may be used to quantify these compounds at the level of 80 μg L(-1), while simultaneous determination of sulfur is very useful for qualitative analysis. Moreover, the results presented in this paper demonstrate the practical applicability of coupling LC with ICP-MS in determining phosphorothioate oligonucleotides and their metabolites in serum within 7 min with a very good sensitivity. The method was linear in the concentration range between 0.2 and 3 mg L(-1). The limit of detection was in the range of 0.07 and 0.13 mg L(-1). Accuracy varied with concentration, but was in the range of 3%. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. A new processing scheme for ultra-high resolution direct infusion mass spectrometry data

    Science.gov (United States)

    Zielinski, Arthur T.; Kourtchev, Ivan; Bortolini, Claudio; Fuller, Stephen J.; Giorio, Chiara; Popoola, Olalekan A. M.; Bogialli, Sara; Tapparo, Andrea; Jones, Roderic L.; Kalberer, Markus

    2018-04-01

    High resolution, high accuracy mass spectrometry is widely used to characterise environmental or biological samples with highly complex composition enabling the identification of chemical composition of often unknown compounds. Despite instrumental advancements, the accurate molecular assignment of compounds acquired in high resolution mass spectra remains time consuming and requires automated algorithms, especially for samples covering a wide mass range and large numbers of compounds. A new processing scheme is introduced implementing filtering methods based on element assignment, instrumental error, and blank subtraction. Optional post-processing incorporates common ion selection across replicate measurements and shoulder ion removal. The scheme allows both positive and negative direct infusion electrospray ionisation (ESI) and atmospheric pressure photoionisation (APPI) acquisition with the same programs. An example application to atmospheric organic aerosol samples using an Orbitrap mass spectrometer is reported for both ionisation techniques resulting in final spectra with 0.8% and 8.4% of the peaks retained from the raw spectra for APPI positive and ESI negative acquisition, respectively.

  17. An ultra-high vacuum scanning tunneling microscope operating at sub-Kelvin temperatures and high magnetic fields for spin-resolved measurements

    Science.gov (United States)

    Salazar, C.; Baumann, D.; Hänke, T.; Scheffler, M.; Kühne, T.; Kaiser, M.; Voigtländer, R.; Lindackers, D.; Büchner, B.; Hess, C.

    2018-06-01

    We present the construction and performance of an ultra-low-temperature scanning tunneling microscope (STM), working in ultra-high vacuum (UHV) conditions and in high magnetic fields up to 9 T. The cryogenic environment of the STM is generated by a single-shot 3He magnet cryostat in combination with a 4He dewar system. At a base temperature (300 mK), the cryostat has an operation time of approximately 80 h. The special design of the microscope allows the transfer of the STM head from the cryostat to a UHV chamber system, where samples and STM tips can be easily exchanged. The UHV chambers are equipped with specific surface science treatment tools for the functionalization of samples and tips, including high-temperature treatments and thin film deposition. This, in particular, enables spin-resolved tunneling measurements. We present test measurements using well-known samples and tips based on superconductors and metallic materials such as LiFeAs, Nb, Fe, and W. The measurements demonstrate the outstanding performance of the STM with high spatial and energy resolution as well as the spin-resolved capability.

  18. Metabolite profiling and quantification of phytochemicals in potato extracts using ultra-high-performance liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Chong, Esther Swee Lan; McGhie, Tony K; Heyes, Julian A; Stowell, Kathryn M

    2013-12-01

    Potatoes contain a diverse range of phytochemicals which have been suggested to have health benefits. Metabolite profiling and quantification were conducted on plant extracts made from a white potato cultivar and 'Urenika', a purple potato cultivar traditionally consumed by New Zealand Maori. There is limited published information regarding the metabolite profile of Solanum tuberosum cultivar 'Urenika'. Using ultra-high- performance liquid chromatography-mass spectrometry (UHPLC-MS), a total of 31 compounds were identified and quantified in the potato extracts. The majority of the compounds were identified for the first time in 'Urenika'. These compounds include several types of anthocyanins, hydroxycinnamic acid (HCA) derivatives, and hydroxycinnamic amides (HCAA). Six classes of compounds, namely organic acids, amino acids, HCA, HCAA, flavonols and glycoalkaloids, were present in both extracts but quantities varied between the two extracts. The unknown plant metabolites in both potato extracts were assigned with molecular formulae and identified with high confidence. Quantification of the metabolites was achieved using a number of appropriate standards. High-resolution mass spectrometry data critical for accurate identification of unknown phytochemicals were achieved and could be added to potato or plant metabolomic database. © 2013 Society of Chemical Industry.

  19. Oligomers, organosulfates, and nitrooxy organosulfates in rainwater identified by ultra-high resolution electrospray ionization FT-ICR mass spectrometry

    Directory of Open Access Journals (Sweden)

    K. E. Altieri

    2009-04-01

    Full Text Available Wet deposition is an important removal mechanism for atmospheric organic matter, and a potentially important input for receiving ecosystems, yet less than 50% of rainwater organic matter is considered chemically characterized. Precipitation samples collected in New Jersey, USA, were analyzed by negative ion ultra-high resolution electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS. Elemental compositions of 552 unique molecular species were determined in the mass range 50–500 Da in the rainwater. Four main groups of organic compounds were identified: compounds containing carbon, hydrogen, and oxygen (CHO only, sulfur (S containing CHOS compounds, nitrogen (N containing CHON compounds, and S- and N- containing CHONS compounds. Organic acids commonly identified in precipitation were detected in the rainwater. Within the four main groups of compounds detected in the rainwater, oligomers, organosulfates, and nitrooxy-organosulfates were assigned based on elemental formula comparisons. The majority of the compounds identified are products of atmospheric reactions and are known contributors to secondary organic aerosol (SOA formed from gas phase, aerosol phase, and in-cloud reactions in the atmosphere. It is suggested that the large uncharacterized component of SOA is the main contributor to the large uncharacterized component of rainwater organic matter.

  20. [Determination of thyreostats in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Lech, Rodziewicz; Jolanta, MasŁOwiecka; Anna, Sadowska; Halina, Car

    2017-10-08

    Five thyreostats (TSs), namely tapazole, thiouracil, methylthiouracil, propylthiouracil, and phenylthiouracil, were determined in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) in positive electrospray ionization mode. Extraction and clean-up were achieved using a ChemElut cartridge with tert -butyl methyl ether, without a derivatization step. Separation was achieved on an Acquity UPLC SS T3 column. The mobile phase was acetonitrile and water containing 0.2% (v/v) formic acid. The mass spectrometer was operated in multiple reaction monitoring mode. Urine samples were spiked with TS solution at levels corresponding to 5, 10, 15, and 20 μg/L. The accuracy (internal standard corrected) ranged from 92% to 107%, with a repeatability precision (relative standard deviation, RSD) less than 15% for all five analytes. The RSDs within-laboratory reproducibility was less than 26%. The decision limits (CCα) and detection capabilities (CCβ) were obtained from a calibration curve and were in the ranges of 3.1-6.1 μg/L and 4.0-7.4 μg/L, respectively. The CCα and CCβ values were below the recommended concentration, which was set at 10 μg/L. The results show that the described method is suitable for the direct detection of TSs in bovine urine. This method can also be used to determine TSs in porcine urine.

  1. Metabolic profiling of Hoodia, Chamomile, Terminalia Species and evaluation of commercial preparations using Ultra-High Performance Quadrupole Time of Flight-Mass Spectrometry

    Science.gov (United States)

    Ultra-High Performance-Quadrupole Time of Flight Mass Spectrometr(UHPLC-QToF-MS)profiling has become an impattant tool for identification of marker compounds and generation of metabolic patterns that could be interrogated using chemometric modeling software. Chemometric approaches can be used to ana...

  2. Characterisation of chemical components for identifying historical Chinese textile dyes by ultra high performance liquid chromatography – photodiode array – electrospray ionisation mass spectrometer

    NARCIS (Netherlands)

    Han, J.; Wanrooij, J.; van Bommel, M.; Quye, A.

    2017-01-01

    This research makes the first attempt to apply Ultra High Performance Liquid Chromatography (UHPLC) coupled to both Photodiode Array detection (PDA) and Electrospray Ionisation Mass Spectrometer (ESI–MS) to the chemical characterisation of common textile dyes in ancient China. Three different

  3. Ultra-high-performance liquid chromatography-tandem mass spectrometry measurement of climbazole deposition from hair care products onto artificial skin and human scalp

    NARCIS (Netherlands)

    Chen, G.; Hoptroff, M.; Fei, X.; Su, Y.; Janssen, H.-G.

    2013-01-01

    A sensitive and specific ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated for the measurement of climbazole deposition from hair care products onto artificial skin and human scalp. Deuterated climbazole was used as the internal

  4. Development and optimization of ultra-high performance supercritical fluid chromatography mass spectrometry method for high-throughput determination of tocopherols and tocotrienols in human serum

    Czech Academy of Sciences Publication Activity Database

    Pilařová, V.; Gottvald, T.; Svoboda, P.; Novák, Ondřej; Benešová, K.; Běláková, S.; Nováková, L.

    2016-01-01

    Roč. 934, AUG 31 (2016), s. 252-265 ISSN 0003-2670 R&D Projects: GA MŠk(CZ) LO1204 Institutional support: RVO:61389030 Keywords : Ultra-high performance supercritical fluid chromatography * Mass spectrometry * Liquid liquid extraction Subject RIV: EB - Genetics ; Molecular Biology Impact factor: 4.950, year: 2016

  5. The use of ultra-high pressure liquid chromatography with tandem mass spectrometric detection of analysis of agrochemical residues and mycotoxines in food - challenges and applications

    Science.gov (United States)

    In the field of food contaminant analysis, the most significant development of recent years has been the integration of ultra-high pressure liquid chromatography (UHPLC), coupled to tandem quadrupole mass spectrometry (MS/MS), into analytical applications. In this review, we describe the emergence o...

  6. Dynamics of laser mass-limited foil interaction at ultra-high laser intensities

    Energy Technology Data Exchange (ETDEWEB)

    Yu, T. P., E-mail: tongpu@nudt.edu.cn [College of Science, National University of Defense Technology, Changsha 410073 (China); State Key Laboratory of High Performance Computing, National University of Defense Technology, Changsha 410073 (China); Sheng, Z. M. [Key Laboratory for Laser Plasmas (MoE) and Department of Physics, Shanghai Jiao Tong University, Shanghai 200240 (China); SUPA, Department of Physics, University of Strathclyde, Glasgow G4 0NG (United Kingdom); Yin, Y.; Zhuo, H. B.; Ma, Y. Y.; Shao, F. Q. [College of Science, National University of Defense Technology, Changsha 410073 (China); Pukhov, A. [Institut für Theoretische Physik I, Heinrich-Heine-Universität Düsseldorf, 40225 Düsseldorf (Germany)

    2014-05-15

    By using three-dimensional particle-in-cell simulations with synchrotron radiation damping incorporated, dynamics of ultra-intense laser driven mass-limited foils is presented. When a circularly polarized laser pulse with a peak intensity of ∼10{sup 22} W/cm{sup 2} irradiates a mass-limited nanofoil, electrons are pushed forward collectively and a strong charge separation field forms which acts as a “light sail” and accelerates the protons. When the laser wing parts overtake the foil from the foil boundaries, electrons do a betatron-like oscillation around the center proton bunch. Under some conditions, betatron-like resonance takes place, resulting in energetic circulating electrons. Finally, bright femto-second x rays are emitted in a small cone. It is also shown that the radiation damping does not alter the foil dynamics radically at considered laser intensities. The effects of the transverse foil size and laser polarization on x-ray emission and foil dynamics are also discussed.

  7. Simultaneous determination of mushroom toxins α-amanitin, β-amanitin and muscarine in human urine by solid-phase extraction and ultra-high-performance liquid chromatography coupled with ultra-high-resolution TOF mass spectrometry.

    Science.gov (United States)

    Tomková, Jana; Ondra, Peter; Válka, Ivo

    2015-06-01

    This paper presents a method for the simultaneous determination of α-amanitin, β-amanitin and muscarine in human urine by solid-phase extraction (SPE) and ultra-high-performance liquid chromatography coupled with ultra-high-resolution TOF mass spectrometry. The method can be used for a diagnostics of mushroom poisonings. Different SPE cartridges were tested for sample preparation, namely hydrophilic modified reversed-phase (Oasis HLB) and polymeric weak cation phase (Strata X-CW). The latter gave better results and therefore it was chosen for the subsequent method optimization and partial validation. In the course of validation, limits of detection, linearity, intraday and interday precisions and recoveries were evaluated. The obtained LOD values of α-amanitin and β-amanitin were 1ng/mL and of muscarine 0.09ng/mL. The intraday and interday precisions of human urine spiked with α-amanitin (10ng/mL), β-amanitin (10ng/mL) and muscarine (1ng/mL) ranged from 6% to 10% and from 7% to 13%, respectively. The developed method was proved to be a relevant tool for the simultaneous determination of the studied mushroom toxins in human urine after mushroom poisoning. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

  8. Multiclass determination of phytochemicals in vegetables and fruits by ultra high performance liquid chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Alarcón-Flores, María Isabel; Romero-González, Roberto; Vidal, José Luis Martínez; Frenich, Antonia Garrido

    2013-11-15

    In this study a simultaneous determination of several classes of phytochemicals (isoflavones, glucosinolates, flavones, flavonols and phenolic acids) in tomato, broccoli, carrot, eggplant and grape has been carried out by ultra high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Solid-liquid extraction assisted by rotary agitator was utilised, using a mixture of methanol:water (80:20, v/v) as solvent. The analytical procedure was validated in all the matrices, obtaining recoveries ranging from 60% to 120% with repeatability values (expressed as relative standard deviations, RSDs) lower than 25%. Limits of quantification (LOQs) were always equal or lower than 50μg/kg, except for some glucosinolates (125μg/kg). Finally the method was applied to different matrices such as tomato, broccoli, carrot, grape and eggplant, observing that chlorogenic acid was detected in most of the samples at higher concentrations in relation to the other compounds. Copyright © 2013 Elsevier Ltd. All rights reserved.

  9. Metabolite Analysis of Toosendanin by an Ultra-High Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry Technique

    Directory of Open Access Journals (Sweden)

    Na Li

    2013-09-01

    Full Text Available Toosendanin is the major bioactive component of Melia toosendan Sieb. et Zucc., which is traditionally used for treatment of abdominal pain and as an insecticide. Previous studies reported that toosendanin possesses hepatotoxicity, but the mechanism remains unknown. Its bioavailability in rats is low, which indicates the hepatotoxicity might be induced by its metabolites. In this connection, in the current study, we examined the metabolites obtained by incubating toosendanin with human live microsomes, and then six of these metabolites (M1–M6 were identified for the first time by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry (UHPLC-Q-TOF/MS. Further analysis on the MS spectra showed M1, M2, and M3 are oxidative products and M6 is a dehydrogenation product, while M4 and M5 are oxidative and dehydrogenation products of toosendanin. Moreover, their possible structures were deduced from the MS/MS spectral features. Quantitative analysis demonstrated that M1-M5 levels rapidly increased and reached a plateau at 30 min, while M6 rapidly reached a maximal level at 20 min and then decreased slowly afterwards. These findings have provided valuable data not only for understanding the metabolic fate of toosendanin in liver microsomes, but also for elucidating the possible molecular mechanism of its hepatotoxicity.

  10. Simultaneous determination of ten illegal azo dyes in feed by ultra-high performance liquid chromatography tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Piątkowska Marta

    2017-09-01

    Full Text Available Introduction: The paper presents the method of simultaneous determination of 10 illegal azo dyes in feed by ultra-high performance liquid chromatography coupled with tandem mass spectrometry technique. Material and Methods: The dyes were extracted with hexane, evaporated to dryness, and analysed. Separation was achieved in 7 min in a gradient elution using acetonitrile (A and 0.1% formic acid (B as a mobile phase. Results: The validation results showed the repeatability of the method, which was evaluated at three levels (50, 500, and 5,000 μg/kg. All the matrix calibration curves for the working ranges were linear (R2 0.9904 to 1.0, the repeatability was between 2.1% and 24%, and recoveries ranged from 77.9% to 120%. The LOD and LOQ were at 1-2 and 5-10 μg/kg for different dyes, respectively. Furthermore, the method was applied in the homogeneity tests of the in-house prepared feed containing Sudan I at the levels of 0.5, 5, and 50 mg/kg. Conclusions: A sensitive, selective, and fast multiresidue method was successfully developed and validated. Its robustness was confirmed by the analysis of an experimental feed containing Sudan I.

  11. Ultra-high performance liquid chromatography tandem high-resolution mass spectrometry study of tricyclazole photodegradation products in water.

    Science.gov (United States)

    Gosetti, Fabio; Chiuminatto, Ugo; Mazzucco, Eleonora; Mastroianni, Rita; Bolfi, Bianca; Marengo, Emilio

    2015-06-01

    This paper reports the study of the photodegradation reactions that tricyclazole can naturally undergo, under the action of sunlight, in aqueous solutions of standard tricyclazole and of the commercial BEAM(TM) formulation. The analyses are carried out by ultra-high performance liquid chromatography technique coupled with high-resolution tandem mass spectrometry. Analysis of both tricyclazole and BEAM(TM) water solutions undergone to hydrolysis does not evidence new chromatographic peaks with respect to the not treated solutions. On the contrary, analysis of the same samples subjected to sunlight irradiation shows a decreased intensity of tricyclazole signal and the presence of new chromatographic peaks. Two photodegradation products of tricyclazole have been identified, one of which has been also quantified, being the commercial standard available. The pattern is similar for the solutions of the standard fungicide and of the BEAM(TM) formulation. The results obtained from eco-toxicological tests show that toxicity of tricyclazole standard solutions is greater than that of the irradiated ones, whereas toxicity levels of all the BEAM(TM) solutions investigated (non-irradiated, irradiated, and hydrolyzed) are comparable and lower than those shown by tricyclazole standard solutions. Experiments performed in paddy water solution show that there is no difference in the degradation products formed.

  12. Multi-residue determination of 210 drugs in pork by ultra-high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Yin, Zhiqiang; Chai, Tingting; Mu, Pengqian; Xu, Nana; Song, Yue; Wang, Xinlu; Jia, Qi; Qiu, Jing

    2016-09-09

    This paper presents a multi-residue analytical method for 210 drugs in pork using ultra-high-performance liquid chromatography-Q-Trap tandem mass spectrometry (UPLC-MS/MS) within 20min via positive ESI in scheduled multi-reaction monitoring (MRM) mode. The 210 drugs, belonging to 21 different chemical classes, included macrolides, sulfonamides, tetracyclines, β-lactams, β-agonists, aminoglycosides, antiviral drugs, glycosides, phenothiazine, protein anabolic hormones, non-steroidal anti-inflammatory drugs (NSAIDs), quinolones, antifungal drugs, corticosteroids, imidazoles, piperidines, piperazidines, insecticides, amides, alkaloids and others. A rapid and simple preparation method was applied to process the animal tissues, including solvent extraction with an acetonitrile/water mixture (80/20, v/v), defatting and clean-up processes. The recoveries ranged from 52% to 130% with relative standard deviations (RSDs)<20% for spiked concentrations of 10, 50 and 250μg/kg. More than 90% of the analytes achieved low limits of quantification (LOQs)<10μg/kg. The decision limit (CCα), detection capability (CCβ) values were in the range of 2-502μg/kg and 4-505μg/kg, respectively. This method is significant for food safety monitoring and controlling veterinary drug use. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Determination of pharmaceutical and illicit drugs in oral fluid by ultra-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Di Corcia, D; Lisi, S; Pirro, V; Gerace, E; Salomone, A; Vincenti, M

    2013-05-15

    A simple and extremely fast procedure for the quantitative determination in oral fluid samples of 44 substances, including the most common drugs of abuse and several pharmaceutical drugs, was developed and fully validated. Preliminary sample treatment was limited to protein precipitation. The resulting acetonitrile solution was directly injected into an ultra-high performance liquid chromatograph (UHPLC) equipped with a C18 column (100mm×2.1mm, 1.7μm). The mobile phase eluted with linear gradient (water/formic acid 5mM: acetonitrile/formic acid 5mM; v:v) from 98:2 to 0:100 in 5.0min, followed by isocratic elution at 100% B for 1.0min. The flow rate was 0.6mL/min and the total run time was 9.0min including re-equilibration at the initial conditions. The analytes were revealed by a triple quadrupole mass spectrometer operating in the selected reaction monitoring mode. The method proved to be simple, accurate, rapid and highly sensitive, allowing the simultaneous detection of all compounds. The ease of sample treatment, together with the wide range of detectable substances, all with remarkable analytical sensitivity, make this procedure ideal for the screening of large populations in several forensic and clinical contexts, whenever oral fluid sampling has to be preferred to blood sampling, as for example in short retrospective investigations. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. Ultra-high-performance liquid chromatography-Time-of-flight high resolution mass spectrometry to quantify acidic drugs in wastewater.

    Science.gov (United States)

    Becerra-Herrera, Mercedes; Honda, Luis; Richter, Pablo

    2015-12-04

    A novel analytical approach involving an improved rotating-disk sorptive extraction (RDSE) procedure and ultra-high-performance liquid chromatography (UHPLC) coupled to an ultraspray electrospray ionization source (UESI) and time-of-flight mass spectrometry (TOF/MS), in trap mode, was developed to identify and quantify four non-steroidal anti-inflammatory drugs (NSAIDs) (naproxen, ibuprofen, ketoprofen and diclofenac) and two anti-cholesterol drugs (ACDs) (clofibric acid and gemfibrozil) that are widely used and typically found in water samples. The method reduced the amount of both sample and reagents used and also the time required for the whole analysis, resulting in a reliable and green analytical strategy. The analytical eco-scale was calculated, showing that this methodology is an excellent green analysis, increasing its ecological worth. The detection limits (LOD) and precision (%RSD) were lower than 90ng/L and 10%, respectively. Matrix effects and recoveries were studied using samples from the influent of a wastewater treatment plant (WWTP). All the compounds exhibited suppression of their signals due to matrix effects, and the recoveries were approximately 100%. The applicability and reliability of this methodology were confirmed through the analysis of influent and effluent samples from a WWTP in Santiago, Chile, obtaining concentrations ranging from 1.1 to 20.5μg/L and from 0.5 to 8.6μg/L, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Determination of naphthalene-derived compounds in apples by ultra-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Esparza, X; Moyano, E; Cosialls, J R; Galceran, M T

    2013-06-11

    Naphthylacetic acid, naphthyloxy acetic acid and naphthylacetamide belong to a group of synthetic substances known as "auxin-like" compounds which are used as growth regulators in vegetables and fruits due to their structure similarities with the indoleacetic acid, the most important plant auxin. This paper reports a selective, sensitive and fast ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for the determination of naphthylacetamide (NAD) and the isomers (α and β) of naphthylacetic acid (NAA) and naphthyloxy acetic (NOA) acid in apple samples. A baseline separation between the respective isomers was achieved using an RP-Amide column with gradient elution. The UHPLC-MS/MS method developed, using electrospray and selected reaction monitoring (SRM) acquisition mode led to a reliable determination of these family of compounds in apple samples at low quantitation levels, down to 1.0 μg kg(-1) and 0.25 μg kg(-1) respectively. For confirmation of NAA accurate mass measurement is proposed giving at these conditions quantitation limits of 10 μg kg(-1) for this compound. The UHPLC-MS/MS method developed was used for the analysis of apple samples harvested in three different apple fields from Lleida (Spain) during the blooming period. NAD and NAA were found in samples collected during 4-5 weeks after application at concentrations between the quantification limits and 43 μg kg(-1) and 24 μg kg(-1), respectively. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Molecular characterization of water soluble organic nitrogen in marine rainwater by ultra-high resolution electrospray ionization mass spectrometry

    Directory of Open Access Journals (Sweden)

    K. E. Altieri

    2012-04-01

    Full Text Available Atmospheric water soluble organic nitrogen (WSON is a subset of the complex organic matter in aerosols and rainwater, which impacts cloud condensation processes and aerosol chemical and optical properties and may play a significant role in the biogeochemical cycle of N. However, its sources, composition, connections to inorganic N, and variability are largely unknown. Rainwater samples were collected on the island of Bermuda (32.27° N, 64.87° W, which experiences both anthropogenic and marine influenced air masses. Samples were analyzed by ultra-high resolution electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry to chemically characterize the WSON. Elemental compositions of 2281 N containing compounds were determined over the mass range m/z+ 50 to 500. The five compound classes with the largest number of elemental formulas identified, in order from the highest number of formulas to the lowest, contained carbon, hydrogen, oxygen, and nitrogen (CHON+, CHON compounds that contained sulfur (CHONS+, CHON compounds that contained phosphorus (CHONP+, CHON compounds that contained both sulfur and phosphorus (CHONSP+, and compounds that contained only carbon, hydrogen, and nitrogen (CHN+. Compared to rainwater collected in the continental USA, average O:C ratios of all N containing compound classes were lower in the marine samples whereas double bond equivalent values were higher, suggesting a reduced role of secondary formation mechanisms. Despite their prevalence in continental rainwater, no organonitrates or nitrooxy-organosulfates were detected, but there was an increased presence of organic S and organic P containing compounds in the marine rainwater. Cluster analysis showed a clear chemical distinction between samples collected during the cold season (October to March which have anthropogenic air mass origins and samples collected during the warm season (April to September with remote

  17. Optimisation of pressurized liquid extraction using a multivariate chemometric approach for the determination of anticancer drugs in sludge by ultra high performance liquid chromatography-tandem mass spectrometry

    OpenAIRE

    Seira , Jordan; Claparols , Catherine; Joannis-Cassan , Claire; Albasi , Claire; Montréjaud-Vignoles , Mireille; Sablayrolles , Caroline

    2013-01-01

    International audience; The present paper describes an analytical method for the determination of 2 widely administered anticancer drugs, ifosfamide and cyclophosphamide, contained in sewage sludge. The method relies on the extraction from the solid matrix by pressurized liquid extraction, sample purification by solid-phase extraction and analysis by ultra high performance liquid chromatography coupled with tandem mass spectrometry. The different parameters affecting the extraction efficiency...

  18. A novel strategy for the determination of polycyclic aromatic hydrocarbon monohydroxylated metabolites in urine using ultra-high-performance liquid chromatography with tandem mass spectrometry.

    Czech Academy of Sciences Publication Activity Database

    Lanková, D.; Urbancová, K.; Šrám, Radim; Hajslová, J.; Pulkrabová, J.

    2016-01-01

    Roč. 408, č. 10 (2016), s. 2515-2525 ISSN 1618-2642 R&D Projects: GA ČR(CZ) GA13-13458S Institutional support: RVO:68378041 Keywords : monohydroxylated metabolites of polycyclic aromatic hydrocarbons * SRM 3673 * tandem mass spectrometry * ultra-high-performance liquid chromatography * urine Subject RIV: DN - Health Impact of the Environment Quality Impact factor: 3.431, year: 2016

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

    Science.gov (United States)

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

    2014-11-01

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

  20. Food contaminant analysis at ultra-high mass resolution: application of hybrid linear ion trap - orbitrap mass spectrometry for the determination of the polyether toxins, azaspiracids, in shellfish.

    LENUS (Irish Health Repository)

    2010-10-30

    The biotoxins, azaspiracids (AZAs), from marine phytoplankton accumulate in shellfish and affect human health by causing severe gastrointestinal disturbance, diarrhea, nausea and vomiting. Specific and sensitive methods have been developed and validated for the determination of the most commonly occurring azaspiracid analogs. An LTQ Orbitrap mass spectrometer is a hybrid instrument that combines linear ion trap (LIT) mass spectrometry (MS) with high-resolution Fourier transform (FT) MS and this was exploited to perform simultaneous ultra-high-resolution full-scan MS analysis and collision-induced dissociation (CID) tandem mass spectrometry (MS\\/MS). Using the highest mass resolution setting (100,000 FWHM) in full-scan mode, the methodology was validated for the determination of six AZAs in mussel (Mytilus galloprovincialis) tissue extracts. Ultra-high mass resolution, together with a narrow mass tolerance window of ±2 mDa, dramatically improved detection sensitivity. In addition to employing chromatographic resolution to distinguish between the isomeric azaspiracid analogs, AZA1\\/AZA6 and AZA4\\/AZA5, higher energy collisionally induced dissociation (HCD) fragmentation on selected precursor ions were performed in parallel with full-scan FTMS. Using HCD MS\\/MS, most precursor and product ion masses were determined within 1 ppm of the theoretical m\\/z values throughout the mass spectral range and this enhanced the reliability of analyte identity.For the analysis of mussels (M. galloprovincialis), the method limit of quantitation (LOQ) was 0.010 µg\\/g using full-scan FTMS and this was comparable with the LOQ (0.007 µg\\/g) using CID MS\\/MS. The repeatability data were; intra-day RSD% (1.8-4.4%; n = 6) and inter-day RSD% (4.7-8.6%; n = 3). Application of these methods to the analysis of mussels (M. edulis) that were naturally contaminated with azaspiracids, using high-resolution full-scan Orbitrap MS and low-resolution CID MS\\/MS, produced

  1. Ultra-high performance supercritical fluid chromatography-mass spectrometry procedure for analysis of monosaccharides from plant gum binders.

    Science.gov (United States)

    Pauk, Volodymyr; Pluháček, Tomáš; Havlíček, Vladimír; Lemr, Karel

    2017-10-09

    The ultra-high performance supercritical fluid chromatography-mass spectrometry (UHPSFC/MS) procedure for analysis of native monosaccharides was developed. Chromatographic conditions were investigated to separate a mixture of four hexoses, three pentoses, two deoxyhexoses and two uronic acids. Increasing water content in methanol modifier to 5% and formic acid to 4% improved peak shapes of neutral monosaccharides and allowed complete elution of highly polar uronic acids in a single run. An Acquity HSS C18SB column outperformed other three tested stationary phases (BEH (silica), BEH 2-ethylpyridine, CSH Fluoro-Phenyl) in terms of separation of isomers and analysis time (4.5 min). Limits of detection were in the range 0.01-0.12 ng μL -1 . Owing to separation of anomers, identification of critical pairs (arabinose-xylose and glucose-galactose) was possible. Feasibility of the new method was demonstrated on plant-derived polysaccharide binders. Samples of watercolor paints, painted paper and three plant gums widely encountered in painting media (Arabic, cherry and tragacanth) were decomposed prior the analysis by microwave-assisted hydrolysis at 40 bar initial pressure using 2 mol L -1 trifluoroacetic acid. Among tested temperatures, 120 °C ensured appropriate hydrolysis efficiency for different types of gum and avoided excessive degradation of labile monosaccharides. Procedure recovery tested on gum Arabic was 101% with an RSD below 8%. Aqueous hydrolysates containing monosaccharides in different ratios specific to each type of plant gum were diluted or analyzed directly. Filtration of samples before hydrolysis reduced interferences from a paper support and identification of gum Arabic in watercolor-painted paper samples was demonstrated. Successful identification of pure gum Arabic was confirmed for sample quantities as little as 1 μg. Two classification approaches were compared and principal component analysis was superior to analysis based on peak area

  2. Ultra high performance liquid chromatography tandem mass spectrometry determination and profiling of prohibited steroids in human biological matrices. A review.

    Science.gov (United States)

    Gosetti, Fabio; Mazzucco, Eleonora; Gennaro, Maria Carla; Marengo, Emilio

    2013-05-15

    list of the prohibited substances of the World Anti-Doping Agency (WADA). In WADA list steroids figure in three main classes, namely anabolic steroids, corticosteroids and substances with anti-estrogenic properties. It must be strongly reminded that assumption of doping agents not only leads to athletes the possible failing of doping tests but causes important health risk and WADA prohibited list establishes criteria to highlight the alteration of the natural steroid profile caused by exogenous administration. Doping control analyses are generally performed in urine, a matrix that provides a prolonged detection time window, and less often in blood, serum, plasma, hair, saliva, and nails. To identify the chemical structures of anabolic steroids the use of mass spectrometry detection is very advantageous. Gas chromatography-mass spectrometry (GC-MS) techniques allowed for the development of comprehensive screening methods. GC-MS methods are sensitive and robust but present the disadvantages of time-consuming sample pretreatment, that is often based on hydrolysis and derivatisation reactions. Liquid chromatography-mass spectrometry (LC-MS) methods have been successfully used to identify and determinate steroids in different matrices, as well as to study their metabolisms. Nowadays, automatic rapid ultra high performance liquid chromatography (UHPLC) tandem mass spectrometry has become the technique of choice for steroid analysis. Due to its generally higher speed, sensitivity, reproducibility and specificity with respect to HPLC, it can be used to simultaneously separate and determinate multi component steroid mixtures. The technique is of huge interest to separate conjugates anabolic androgenic steroids, as it allows efficiency enhancement due to the small particle (sub-2μm) column packing, which provides high peak capacity within analysis times even 5-10 fold shorter than conventional HPLC methods. Modern multiplex instruments can analyze thousands of samples per month

  3. Study of dispersion of mass distribution of ultra-high energy cosmic rays using a surface array of muon and electromagnetic detectors

    Science.gov (United States)

    Vícha, Jakub; Trávníček, Petr; Nosek, Dalibor; Ebr, Jan

    2015-09-01

    We consider a hypothetical observatory of ultra-high energy cosmic rays consisting of two surface detector arrays that measure independently electromagnetic and muon signals induced by air showers. Using the constant intensity cut method, sets of events ordered according to each of both signal sizes are compared giving the number of matched events. Based on its dependence on the zenith angle, a parameter sensitive to the dispersion of the distribution of the logarithmic mass of cosmic rays is introduced. The results obtained using two post-LHC models of hadronic interactions are very similar and indicate a weak dependence on details of these interactions.

  4. Highly informative multiclass profiling of lipids by ultra-high performance liquid chromatography - Low resolution (quadrupole) mass spectrometry by using electrospray ionization and atmospheric pressure chemical ionization interfaces.

    Science.gov (United States)

    Beccaria, Marco; Inferrera, Veronica; Rigano, Francesca; Gorynski, Krzysztof; Purcaro, Giorgia; Pawliszyn, Janusz; Dugo, Paola; Mondello, Luigi

    2017-08-04

    A simple, fast, and versatile method, using an ultra-high performance liquid chromatography system coupled with a low resolution (single quadrupole) mass spectrometer was optimized to perform multiclass lipid profiling of human plasma. Particular attention was made to develop a method suitable for both electrospray ionization and atmospheric pressure chemical ionization interfaces (sequentially in positive- and negative-ion mode), without any modification of the chromatographic conditions (mobile phase, flow-rate, gradient, etc.). Emphasis was given to the extrapolation of the structural information based on the fragmentation pattern obtained using atmospheric pressure chemical ionization interface, under each different ionization condition, highlighting the complementary information obtained using the electrospray ionization interface, of support for related molecule ions identification. Furthermore, mass spectra of phosphatidylserine and phosphatidylinositol obtained using the atmospheric pressure chemical ionization interface are reported and discussed for the first time. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Metabolite characterization of a novel sedative drug, remimazolam in human plasma and urine using ultra high-performance liquid chromatography coupled with synapt high-definition mass spectrometry.

    Science.gov (United States)

    Zhou, Ying; Hu, Pei; Jiang, Ji

    2017-04-15

    Remimazolam is a new chemical entity belonging to the benzodiazepine class of sedative drugs, which shows faster-acting onset and recovery than currently available short-acting sedatives. In the present study, ultra high performance liquid chromatography with synapt high-definition mass spectrometry method combined with MassLynx software was established to characterize metabolites of remimazolam in human plasma and urine. In total, 5 human metabolites were detected, including 3 phase I and 2 phase II metabolites. There was no novel human metabolite detected compared to that in rat. Hydrolysis, glucuronidation and oxidation were the major metabolic reactions. To our knowledge, this is the first report of the human metabolic profile of remimazolam. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. The utility of ultra-high performance supercritical fluid chromatography-tandem mass spectrometry (UHPSFC-MS/MS) for clinically relevant steroid analysis.

    Science.gov (United States)

    Storbeck, Karl-Heinz; Gilligan, Lorna; Jenkinson, Carl; Baranowski, Elizabeth S; Quanson, Jonathan L; Arlt, Wiebke; Taylor, Angela E

    2018-05-15

    Liquid chromatography tandem mass spectrometry (LC-MS/MS) assays are considered the reference standard for serum steroid hormone analyses, while full urinary steroid profiles are only achievable by gas chromatography (GC-MS). Both LC-MS/MS and GC-MS have well documented strengths and limitations. Recently, commercial ultra-high performance supercritical fluid chromatography-tandem mass spectrometry (UHPSFC-MS/MS) systems have been developed. These systems combine the resolution of GC with the high-throughput capabilities of UHPLC. Uptake of this new technology into research and clinical labs has been slow, possibly due to the perceived increase in complexity. Here we therefore present fundamental principles of UHPSFC-MS/MS and the likely applications for this technology in the clinical research setting, while commenting on potential hurdles based on our experience to date. Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.

  7. Profiling of nonvolatiles in whiskeys using ultra high pressure liquid chromatography quadrupole time-of-flight mass spectrometry (UHPLC-QTOF MS).

    Science.gov (United States)

    Collins, Thomas S; Zweigenbaum, Jerry; Ebeler, Susan E

    2014-11-15

    Commercial samples of 63 American whiskeys, including bourbon whiskeys, Tennessee whiskeys, rye whiskeys and other blended whiskeys were analysed using ultra high pressure liquid chromatography (UHPLC) coupled with quadrupole time-of-flight (QTOF) mass spectrometry (MS). The non-volatile composition of the whiskeys was used to model differences among the samples using discriminant analysis. The blended American whiskeys were readily distinguished from the remaining types. Additionally, most Tennessee whiskeys could be differentiated from bourbon and rye whiskeys. Similarly, younger (8 years old) whiskeys could be separated. The compounds important for differentiating among these whiskeys included wood derived phenolic compounds, lignan derived compounds and several C8 and larger lipids. A number of additional compounds differentiated the whiskeys but could not be identified using MS and MS/MS data alone. Copyright © 2014 Elsevier Ltd. All rights reserved.

  8. A multiresidue approach for the simultaneous quantification of antibiotics in macroalgae by ultra-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Leston, Sara; Freitas, Andreia; Rosa, João; Barbosa, Jorge; Lemos, Marco F L; Pardal, Miguel Ângelo; Ramos, Fernando

    2016-10-15

    Together with fish, algae reared in aquaculture systems have gained importance in the last years, for many purposes. Besides their use as biofilters of effluents, macroalgae's rich nutritional profiles have increased their inclusion in human diets but also in animal feeds as sources of fatty acids, especially important for the fish industry. Nonetheless, algae are continuously exposed to environmental contaminants including antibiotics and possess the ability for bioaccumulation of such compounds. Therefore, the present paper describes the development and validation of an ultra-high performance liquid chromatography with tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous quantification of antibiotics in the green macroalgae Ulva lactuca. This multi-residue method enables the determination of 38 compounds distributed between seven classes and was fully validated according to EU Decision 2002/657/EC. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. Qualitative and Quantitative Analysis of Volatile Components of Zhengtian Pills Using Gas Chromatography Mass Spectrometry and Ultra-High Performance Liquid Chromatography.

    Science.gov (United States)

    Liu, Cui-Ting; Zhang, Min; Yan, Ping; Liu, Hai-Chan; Liu, Xing-Yun; Zhan, Ruo-Ting

    2016-01-01

    Zhengtian pills (ZTPs) are traditional Chinese medicine (TCM) which have been commonly used to treat headaches. Volatile components of ZTPs extracted by ethyl acetate with an ultrasonic method were analyzed by gas chromatography mass spectrometry (GC-MS). Twenty-two components were identified, accounting for 78.884% of the total components of volatile oil. The three main volatile components including protocatechuic acid, ferulic acid, and ligustilide were simultaneously determined using ultra-high performance liquid chromatography coupled with diode array detection (UHPLC-DAD). Baseline separation was achieved on an XB-C18 column with linear gradient elution of methanol-0.2% acetic acid aqueous solution. The UHPLC-DAD method provided good linearity (R (2) ≥ 0.9992), precision (RSD components, protocatechuic acid, ferulic acid, and ligustilide, in 13 batches of ZTPs, which is suitable for discrimination and quality assessment of ZTPs.

  10. Rapid Characterization and Identification of Flavonoids in Radix Astragali by Ultra-High-Pressure Liquid Chromatography Coupled with Linear Ion Trap-Orbitrap Mass Spectrometry.

    Science.gov (United States)

    Zhang, Jing; Xu, Xiao-Jie; Xu, Wen; Huang, Juan; Zhu, Da-yuan; Qiu, Xiao-Hui

    2015-07-01

    A simple and effective method was established for separation and characterization of flavonoid constituents in Radix Astragali (RA) by combination of ultra-high-pressure liquid chromatography with LTQ-Orbitrap tandem mass spectrometry (u-HPLC-LTQ-Orbitrap-MS(n)). For three major structural types of flavonoids, the proposed fragmentation pathways and major diagnostic fragment ions of isoflavones, pterocarpans and isoflavans were investigated to trace isoflavonoid derivatives in crude plant extracts. Based on the systematic identification strategy, 48 constituents were rapidly detected and characterized or tentatively identified, many of which were first reported in RA. The u-PHLC-LTQ-Orbitrap MS(n) platform was proved as an effective tool for rapid qualitative analysis of secondary metabolite productions from natural resources. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  11. Validation of a method for simultaneous determination of nitroimidazoles, benzimidazoles and chloramphenicols in swine tissues by ultra-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Xia, Xi; Wang, Yuanyuan; Wang, Xia; Li, Yun; Zhong, Feng; Li, Xiaowei; Huang, Yaoling; Ding, Shuangyang; Shen, Jianzhong

    2013-05-31

    This paper presents a sensitive and confirmatory multi-residue method for the analysis of 23 veterinary drugs and metabolites belonging to three classes (nitroimidazoles, benzimidazoles, and chloramphenicols) in porcine muscle, liver, and kidney. After extracted with ethyl acetate and basic ethyl acetate sequentially, the crude extracts were defatted with hexane and further purified using Oasis MCX solid-phase extraction cartridges. Rapid determination was carried out by ultra-high performance liquid chromatography-electrospray ionization tandem mass spectrometry. Data acquisition was performed under positive and negative mode simultaneously. Recoveries based on matrix-matched calibrations for meat, liver, and kidney ranged from 50.6 to 108.1%. The method quantification limits were in the range of 3-100ng/kg. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. Mass composition studies of Ultra High Energy cosmic rays through the measurement of the Muon Production Depths at the Pierre Auger Observatory

    Energy Technology Data Exchange (ETDEWEB)

    Collica, Laura [Univ. of Milan (Italy); Paris Diderot Univ. (France)

    2014-01-01

    The Pierre Auger Observatory (Auger) in Argentina studies Ultra High Energy Cosmic Rays (UHECRs) physics. The flux of cosmic rays at these energies (above 1018 eV) is very low (less than 100 particle/km2-year) and UHECR properties must be inferred from the measurements of the secondary particles that the cosmic ray primary produces in the atmosphere. These particles cascades are called Extensive Air Showers (EAS) and can be studied at ground by deploying detectors covering large areas. The EAS physics is complex, and the properties of secondary particles depend strongly on the first interaction, which takes place at an energy beyond the ones reached at accelerators. As a consequence, the analysis of UHECRs is subject to large uncertainties and hence many of their properties, in particular their composition, are still unclear. Two complementary techniques are used at Auger to detect EAS initiated by UHE- CRs: a 3000 km2 surface detector (SD) array of water Cherenkov tanks which samples particles at ground level and fluorescence detectors (FD) which collect the ultraviolet light emitted by the de-excitation of nitrogen nuclei in the atmosphere, and can operate only in clear, moonless nights. Auger is the largest cosmic rays detector ever built and it provides high-quality data together with unprecedented statistics. The main goal of this thesis is the measurement of UHECR mass composition using data from the SD of the Pierre Auger Observatory. Measuring the cosmic ray composition at the highest energies is of fundamental importance from the astrophysical point of view, since it could discriminate between different scenarios of origin and propagation of cosmic rays. Moreover, mass composition studies are of utmost importance for particle physics. As a matter of fact, knowing the composition helps in exploring the hadronic interactions at ultra-high energies, inaccessible to present accelerator experiments.

  13. A fast and sensitive method for the separation of carotenoids using ultra-high performance supercritical fluid chromatography-mass spectrometry.

    Science.gov (United States)

    Jumaah, Firas; Plaza, Merichel; Abrahamsson, Victor; Turner, Charlotta; Sandahl, Margareta

    2016-08-01

    In this study, a rapid and sensitive ultra-high performance supercritical fluid chromatography-mass spectrometry (UHPSFC-MS) method has been developed and partially validated for the separation of carotenoids within less than 6 min. Six columns of orthogonal selectivity were examined, and the best separation was obtained by using a 1-aminoanthracene (1-AA) column. The length of polyene chain as well as the number of hydroxyl groups in the structure of the studied carotenoids determines their differences in the physiochemical properties and thus the separation that is achieved on this column. All of the investigated carotenoids were baseline separated with resolution values greater than 1.5. The effects of gradient program, back pressure, and column temperature were studied with respect to chromatographic properties such as retention and selectivity. Electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) were compared in both positive and negative mode, using both direct infusion and hyphenated with UHPSFC. The ESI in positive mode provided the highest response. The coefficient of determination (R (2)) for all calibration curves were greater than 0.998. Limit of detection (LOD) was in the range of 2.6 and 25.2 ng/mL for α-carotene and astaxanthin, respectively, whereas limit of quantification (LOQ) was in the range of 7.8 and 58.0 ng/mL for α-carotene and astaxanthin, respectively. Repeatability and intermediate precision of the developed UHPSFC-MS method were determined and found to be RSD supercritical fluid extracts of microalgae and rosehip. Graphical Abstract Ultra-high performance supercritical fluid chromatography-a rapid separation method for the analysis of carotenoids in rosehip and microalgae samples.

  14. [Screening and confirmation of 24 hormones in cosmetics by ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry].

    Science.gov (United States)

    Li, Zhaoyong; Wang, Fengmei; Niu, Zengyuan; Luo, Xin; Zhang, Gang; Chen, Junhui

    2014-05-01

    A method of ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry (UPLC-LTQ/Orbitrap MS) was established to screen and confirm 24 hormones in cosmetics. Various cosmetic samples were extracted with methanol. The extract was loaded onto a Waters ACQUITY UPLC BEH C18 column (50 mm x 2.1 mm, 1.7 microm) using a gradient elution of acetonitrile/water containing 0.1% (v/v) formic acid for the separation. The accurate mass of quasi-molecular ion was acquired by full scanning of electrostatic field orbitrap. The rapid screening was carried out by the accurate mass of quasi-molecular ion. The confirmation analysis for targeted compounds was performed with the retention time and qualitative fragments obtained by data dependent scan mode. Under the optimal conditions, the 24 hormones were routinely detected with mass accuracy error below 3 x 10(-6) (3 ppm), and good linearities were obtained in their respective linear ranges with correlation coefficients higher than 0.99. The LODs (S/N = 3) of the 24 compounds were hormones in 50 cosmetic samples. The results demonstrate that the method is a useful tool for the rapid screening and identification of the hormones in cosmetics.

  15. A Method to Search for Correlations of Ultra-high Energy Cosmic-Ray Masses with the Large-scale Structures in the Local Galaxy Density Field

    Science.gov (United States)

    Ivanov, A. A.

    2013-02-01

    One of the main goals of investigations using present and future giant extensive air shower (EAS) arrays is the mass composition of ultra-high energy cosmic rays (UHECRs). A new approach to the problem is presented, combining the analysis of arrival directions with the statistical test of the paired EAS samples. One of the ideas of the method is to search for possible correlations between UHECR masses and their separate sources; for instance, if there are two sources in different areas of the celestial sphere injecting different nuclei, but the fluxes are comparable so that arrival directions are isotropic, then the aim is to reveal a difference in the mass composition of cosmic-ray fluxes. The method is based on a non-parametric statistical test—the Wilcoxon signed-rank routine—which does not depend on the populations fitting any parameterized distributions. Two particular algorithms are proposed: first, using measurements of the depth of the EAS maximum position in the atmosphere; and second, relying on the age variance of air showers initiated by different primary particles. The formulated method is applied to the Yakutsk array data, in order to demonstrate the possibility of searching for a difference in average mass composition between the two UHECR sets, arriving particularly from the supergalactic plane and a complementary region.

  16. A METHOD TO SEARCH FOR CORRELATIONS OF ULTRA-HIGH ENERGY COSMIC-RAY MASSES WITH THE LARGE-SCALE STRUCTURES IN THE LOCAL GALAXY DENSITY FIELD

    International Nuclear Information System (INIS)

    Ivanov, A. A.

    2013-01-01

    One of the main goals of investigations using present and future giant extensive air shower (EAS) arrays is the mass composition of ultra-high energy cosmic rays (UHECRs). A new approach to the problem is presented, combining the analysis of arrival directions with the statistical test of the paired EAS samples. One of the ideas of the method is to search for possible correlations between UHECR masses and their separate sources; for instance, if there are two sources in different areas of the celestial sphere injecting different nuclei, but the fluxes are comparable so that arrival directions are isotropic, then the aim is to reveal a difference in the mass composition of cosmic-ray fluxes. The method is based on a non-parametric statistical test—the Wilcoxon signed-rank routine—which does not depend on the populations fitting any parameterized distributions. Two particular algorithms are proposed: first, using measurements of the depth of the EAS maximum position in the atmosphere; and second, relying on the age variance of air showers initiated by different primary particles. The formulated method is applied to the Yakutsk array data, in order to demonstrate the possibility of searching for a difference in average mass composition between the two UHECR sets, arriving particularly from the supergalactic plane and a complementary region.

  17. A METHOD TO SEARCH FOR CORRELATIONS OF ULTRA-HIGH ENERGY COSMIC-RAY MASSES WITH THE LARGE-SCALE STRUCTURES IN THE LOCAL GALAXY DENSITY FIELD

    Energy Technology Data Exchange (ETDEWEB)

    Ivanov, A. A., E-mail: ivanov@ikfia.ysn.ru [Shafer Institute for Cosmophysical Research and Aeronomy, 31 Lenin Avenue, Yakutsk 677980 (Russian Federation)

    2013-02-15

    One of the main goals of investigations using present and future giant extensive air shower (EAS) arrays is the mass composition of ultra-high energy cosmic rays (UHECRs). A new approach to the problem is presented, combining the analysis of arrival directions with the statistical test of the paired EAS samples. One of the ideas of the method is to search for possible correlations between UHECR masses and their separate sources; for instance, if there are two sources in different areas of the celestial sphere injecting different nuclei, but the fluxes are comparable so that arrival directions are isotropic, then the aim is to reveal a difference in the mass composition of cosmic-ray fluxes. The method is based on a non-parametric statistical test-the Wilcoxon signed-rank routine-which does not depend on the populations fitting any parameterized distributions. Two particular algorithms are proposed: first, using measurements of the depth of the EAS maximum position in the atmosphere; and second, relying on the age variance of air showers initiated by different primary particles. The formulated method is applied to the Yakutsk array data, in order to demonstrate the possibility of searching for a difference in average mass composition between the two UHECR sets, arriving particularly from the supergalactic plane and a complementary region.

  18. A new Time-of-Flight mass measurement project for exotic nuclei and ultra-high precision detector development

    Directory of Open Access Journals (Sweden)

    Sun Bao-Hua

    2016-01-01

    Full Text Available The time-of-flight (TOF mass spectrometry (MS, a high-resolution magnetic spectrometer equipped with a fast particle tracking system, is well recognized by its ability in weighing the most exotic nuclei. Currently such TOF-MS can achieve a mass resolution power of about 2×10−4. We show that the mass resolution can be further improved by one order of magnitude with augmented timing and position detectors. We report the progress in developing ultra-fast detectors to be used in TOF-MS.

  19. Ultra high resolution tomography

    Energy Technology Data Exchange (ETDEWEB)

    Haddad, W.S.

    1994-11-15

    Recent work and results on ultra high resolution three dimensional imaging with soft x-rays will be presented. This work is aimed at determining microscopic three dimensional structure of biological and material specimens. Three dimensional reconstructed images of a microscopic test object will be presented; the reconstruction has a resolution on the order of 1000 A in all three dimensions. Preliminary work with biological samples will also be shown, and the experimental and numerical methods used will be discussed.

  20. Identification of metabolites of vindoline in rats using ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Zhang, Yuqian; Sun, Yupeng; Mu, Xiyan; Yuan, Lin; Wang, Qiao; Zhang, Lantong

    2017-08-15

    Vindoline (VDL) is an indole alkaloid, possessing hypoglycemic and vasodilator effects, and it is also the prodrug of many vinca alkaloids. In this paper, we analyzed in vivo (including plasma, urine, bile and faeces) and in vitro metabolic profile of VDL in rat with ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF-MS/MS). The chromatographic separation was performed on a C 18 column with a mobile phase consisted of 3mM ammonium acetate buffer and acetonitrile at a flow rate of 300μL/min. The mass spectral analysis was conducted in a positive electrospray ionization mode, and on-line data acquisition method multiple mass defect filter (MMDF) combined with dynamic background subtraction (DBS) were used in the biological samples analysis to trace all the potential metabolites of VDL. Twenty-five metabolites of VDL were detected by comparing with the blank sample, of which there were 2 sulfate conjugates. These data suggested that the biotransformation of VDL was deacetylation, oxidation, deoxidization, methylation, dealkylation and sulfate conjugation. This study provides useful information for further study of the pharmacology and mechanism of VDL, meanwhile, the research method can be widely applied to speculate structural features of the metabolites of other vinca alkaloids. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Characterization and profiling of phenolic amides from Cortex Lycii by ultra-high performance liquid chromatography coupled with LTQ-Orbitrap mass spectrometry.

    Science.gov (United States)

    Zhang, Jingxian; Guan, Shuhong; Sun, Jianghao; Liu, Tian; Chen, Pei; Feng, Ruihong; Chen, Xin; Wu, Wanying; Yang, Min; Guo, De-An

    2015-01-01

    Cortex Lycii, the root bark of Lycium chinense Mill. or Lycium barbarum L., is a frequently used traditional Chinese medicine. Phytochemical studies have shown that phenolic amides are not only characteristic compounds but also abundant ones in this plant. In the present study, an effective method was developed for structural characterization of phenolic amides from Cortex Lycii by ultra-high performance liquid chromatography coupled with linear ion trap Orbitrap tandem mass spectrometry. The fragmentation of 14 compounds including six cinnamic acid amides, six neolignanamides, and two lignanamides were studied systematically for the first time. It was found that, in the positive ion mode, neutral loss of the tyramide moiety (137 Da) or N-(4-aminobutyl)acetamide moiety (130 Da) were characteristic for these compounds. At least 54 phenolic amides were detected in the extract and 48 of them were characterized, among which 14 known compounds were identified unambiguously by comparing the retention time and mass spectra with those of reference compounds, and 34 components were tentatively identified based on the fragmentation patterns, exact mass, UV spectra, as well as retention time. Fifteen compounds were characterized as potential new ones. Additionally, the developed method was applied to analyze eight batches of samples collected from the northwest of China, and it was found that cinnamic acid amides were the main type of phenolic amides in Cortex Lycii. In conclusion, the identification of these chemicals provided essential data for further phytochemical studies, metabolites identification, and the quality control of Cortex Lycii.

  2. Ultra-high performance liquid chromatography-tandem mass spectrometry in high-throughput confirmation and quantification of 34 anabolic steroids in bovine muscle.

    Science.gov (United States)

    Vanhaecke, Lynn; Vanden Bussche, Julie; Wille, Klaas; Bekaert, Karen; De Brabander, Hubert F

    2011-08-26

    An ultra-high performance liquid chromatography tandem mass spectrometry multi-residue method for the determination of 34 anabolic steroids (10 estrogens including stilbenes, 14 androgens and 10 gestagens) in meat of bovine origin is reported. The extraction and clean-up procedure involved homogenization with methanol, defatting with hexane, liquid/liquid extraction with diethylether and finally SPE clean-up with coupled Si and NH(2) cartridges. The analytes were separated on a 1.9 μm Hypersil Gold column (100×2.1 mm) and quantified on a triple quadrupole mass spectrometer (TSQ Vantage) operating simultaneously in both positive and negative atmospheric pressure chemical ionisation (APCI) modes. This analytical procedure was subsequently validated according to EU criteria (CD 2002/657/EC), resulting in decision limits and detection capabilities ranging between 0.04 and 0.88 μg kg(-1) and 0.12 and 1.9 μg kg(-1), respectively. The method obtained for all, natural and synthetic steroids, adequate precisions and intra-laboratory reproducibilities (relative standard deviation below 20%), and the linearity ranged between 0.991 and 0.999. The performance characteristics fulfill the recommended concentrations fixed by the Community Reference Laboratories. The developed analysis is sensitive, and robust and therefore useful for confirmation and quantification of anabolic steroids for research purposes and residue control programs. Copyright © 2010 Elsevier B.V. All rights reserved.

  3. Simultaneous identification and quantification of bisphenol A and 12 bisphenol analogues in environmental samples using precolumn derivatization and ultra high performance liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Wang, Zhonghe; Yu, Jing; Yao, Jiaxi; Wu, Linlin; Xiao, Hang; Wang, Jun; Gao, Rong

    2018-02-10

    A method for the identification and quantification of bisphenol A and 12 bisphenol analogues in river water and sediment samples combining liquid-liquid extraction, precolumn derivatization, and ultra high-performance liquid chromatography coupled with tandem mass spectrometry was developed and validated. Analytes were extracted from the river water sample using a liquid-liquid extraction method. Dansyl chloride was selected as a derivatization reagent. Derivatization reaction conditions affecting production of the dansyl derivatives were tested and optimized. All the derivatized target compounds were well separated and eluted in 10 min. Dansyl chloride labeled compounds were analyzed using a high-resolution mass spectrometer with electrospray ionization in the positive mode, and the results were confirmed and quantified in the parallel reaction monitoring mode. The method validation results showed a satisfactory level of sensitivity. Linearity was assessed using matrix-matched standard calibration, and good correlation coefficients were obtained. The limits of quantification for the analytes ranged from 0.005 to 0.02 ng/mL in river water and from 0.15 to 0.80 ng/g in sediment. Good reproducibility of the method in terms of intra- and interday precision was achieved, yielding relative standard deviations of less than 10.1 and 11.6%, respectively. Finally, this method was successfully applied to the analysis of real samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Qualitative and Quantitative Analysis of Rhizoma Smilacis glabrae by Ultra High Performance Liquid Chromatography Coupled with LTQ OrbitrapXL Hybrid Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Shao-Dan Chen

    2014-07-01

    Full Text Available Rhizoma Smilacis glabrae, a traditional Chinese medicine (TCM as well as a functional food, has been commonly used for detoxification treatments, relieving dampness and as a diuretic. In order to quickly define the chemical profiles and control the quality of Smilacis glabrae, ultra high performance liquid chromatography coupled with electrospray ionization hybrid linear trap quadrupole orbitrap mass spectrometry (UHPLC-ESI/LTQ-Orbitrap-MS was applied for simultaneous identification and quantification of its bioactive constituents. A total of 56 compounds, including six new compounds, were identified or tentatively deduced on the basis of their retention behaviors, mass spectra, or by comparison with reference substances and literature data. The identified compounds belonged to flavonoids, phenolic acids and phenylpropanoid glycosides. In addition, an optimized UHPLC-ESI/LTQ-Orbitrap-MS method was established for quantitative determination of six marker compounds from five batches. The validation of the method, including linearity, sensitivity (LOQ, precision, repeatability and spike recoveries, was carried out and demonstrated to be satisfied the requirements of quantitative analysis. The results suggested that the established method would be a powerful and reliable analytical tool for the characterization of multi-constituent in complex chemical system and quality control of TCM.

  5. Identification of metabolites of Helicid in vivo using ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Diao, Xinpeng; Liao, Man; Cheng, Xiaoye; Liang, Caijuan; Sun, Yupeng; Zhang, Xia; Zhang, Lantong

    2018-04-18

    Helicid is an active natural aromatic phenolic glycoside ingredient originating from well-known traditional Chinese herb medicine and has the significant effects of sedative hypnosis, anti-inflammatory analgesia and antidepressant. In this study, we analyzed the potential metabolites of Helicid in rats by multiple mass defect filter (MMDF)and dynamic background subtraction (DBS)in ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF-MS). Moreover, we used a novel data processing method 'key product ions (KPIs)' to rapidly detect and identifymetabolites as an assistant tool. MetabolitePilot TM 2.0 software and PeakView TM 2.2 software were used for analyzing metabolites. Twenty metabolites of Helicid (including 15 phase I metabolites and 5 phase II metabolites) were detected by comparing with the blank samples, respectively. Thebiotransformationroute of Helicid was identified as demethylation, oxidation, dehydroxylation, hydrogenation, decarbonylation,glucuronide conjugation and methylation.This is the first study of simultaneously detecting and identifying Helicid metabolism in rats by employing UHPLC-Q-TOF-MS technology. This experiment not only proposed a method for rapidly detecting and identifying metabolites, but also provided useful information for further study of the pharmacology and mechanism of Helicid in vivo. Furthermore, it provided an effective method for the analysis of other aromatic phenolic glycosides metabolic components in vivo. This article is protected by copyright. All rights reserved.

  6. Identification of berberrubine metabolites in rats by using ultra-high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Wang, Kun; Qiao, Miao; Chai, Liwei; Cao, Shijie; Feng, Xinchi; Ding, Liqin; Qiu, Feng

    2018-01-01

    Berberrubine, an isoquinoline alkaloid isolated from many medicinal plants, possesses diverse pharmacological activities, including glucose-lowering, lipid-lowering, anti-inflammatory, and anti-tumor effects. This study aimed to investigate the metabolic profile of berberrubine in vivo. Therefore, a rapid and reliable method using the ultra-high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) and metabolynx™ software with mass defect filter (MDF) technique was developed. Plasma, bile, urine and feces samples were collected from rats after oral administration of berberrubine with a dose of 30.0mg/kg and analyzed to characterize the metabolites of berberrubine in vivo for the first time. A total of 57 metabolites were identified, including 54 metabolites in urine, 39 metabolites in plasma, 28 metabolites in bile and 18 metabolites in feces. The results indicated that demethylenation, reduction, hydroxylation, demethylation, glucuronidation, and sulfation were the major metabolic pathways of berberrubine in vivo. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Metabolomic approaches for orange origin discrimination by ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Díaz, Ramon; Pozo, Oscar J; Sancho, Juan V; Hernández, Félix

    2014-08-15

    In this work, hybrid quadrupole time-of-flight mass spectrometer (QTOF MS) coupled to ultra high performance liquid chromatography (UHPLC) has been used for biomarkers identification for correct authentication of Valencia (Spain) oranges. Differentiation from foreign Argentinean, Brazilian and South African oranges has been carried out using XCMS application and multivariate analysis to UHPLC-(Q)TOF MS data acquired in both, positive and negative ionisation modes. Several markers have been found and corroborated by analysing two seasons samples. A seasonal independent marker was found and its structure elucidated using accurate mass data and MS(E) fragmentation spectrum information. Empirical formula was searched in Reaxys database applying sub-structure filtering from the fragments obtained. Three possible structures were found and citrusin D, a compound present in sweet oranges, has been identified as the most plausible as it fits better with the product ion scan performed for this compound. As a result of data obtained in this work, citrusin D is suggested as a potential marker to distinguish the geographic origin of oranges. Copyright © 2014 Elsevier Ltd. All rights reserved.

  8. [Determination of di (hydrogenated tallow alkyl) dimethyl ammonium compounds in textile auxiliaries by ultra-high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Zhu, Feng

    2015-01-01

    A method has been developed for the determination of di (hydrogenated tallow alkyl) dimethyl ammonium compounds (DHTDMAC) in textile auxiliaries by ultra-high performance liquid chromatography-tandem mass spectrometry. (UPLC-MS/MS). The samples were extracted and diluted with acidified methanol by 5% (v/v) formic acid under ultrasonic assistance. The separation was performed on an Eclipse Plus C18 column (50 mm x 2.1 mm, 1.8 microm) using 0.1% (v/v) formic acid solution and methanol as the mobile phases. Identification and quantification were achieved by UPLC-MS/MS with electrospray ionization (ESI) source in positive ion mode and multiple reaction monitoring (MRM) mode. The results indicated that the calibration curve of DHTDMAC showed good linear relationship between peak area and mass concentration in the range of 10-280 microg/L with the correlation coefficient (r2) of 0.9991. The limit of detection (LOD, S/N=3) and the limit of quantification (LOQ, S/N= 10) of this method were 3 mg/kg and 10 mg/kg, respectively. The average recoveries from three typical textile auxiliary matrices including dispersant, antistatic agent and fabric softener, at three spiked levels were in the range of 97.2%-108.3% with the relative standard deviations (RSDs) of 1.5%-4.6%. The method is sensitive, accurate, simple and effective for the analysis of DHTDMAC in textile auxiliaries.

  9. Direct determination of fatty acid esters of 3-chloro-1, 2-propanediol in edible vegetable oils by isotope dilution - ultra high performance liquid chromatography - triple quadrupole mass spectrometry.

    Science.gov (United States)

    Li, Heli; Chen, Dawei; Miao, Hong; Zhao, Yunfeng; Shen, Jianzhong; Wu, Yongning

    2015-09-04

    A selective and sensitive ultra-high performance liquid chromatography - triple quadrupole mass spectrometry (UHPLC-MS/MS) method coupled with matrix solid phase dispersion (MSPD) extraction was developed for the direct determination of fatty acid esters of 3-chloro-1,2-propanediol (3-MCPD esters) in edible vegetable oils. The method integrated the isotope dilution technique, MSPD extraction and UHPLC - MS/MS analysis with multi-reaction monitoring mode (MRM). Matrix-matched calibration curves showed good linearity within the range of 0.01-10mgL(-1) with the correlation coefficient not less than 0.999. Limits of detection (LODs) and limit of quantification (LOQs) of the 3-MCPD esters fell into the range of 0.0001-0.02mgkg(-1) and 0.0004-0.05mgkg(-1), respectively. The recoveries for the spiked extra virgin olive oils ranged from 94.4% to 108.3%, with the relative standard deviations (RSD) ranging from 0.6% to 10.5%. The method was applied for the oil sample (T2642) of the official Food Analysis Performance Assessment Scheme (FAPAS) in 2014 and other real samples from supermarket, and the results showed that the present method was comparative to the gas chromatography-mass spectrometry (GC-MS) method based on the improved German Society for Fat Science (DGF) standard method C-III 18 (09) except for palm oil. Copyright © 2015. Published by Elsevier B.V.

  10. Characterization of polyoxyethylene tallow amine surfactants in technical mixtures and glyphosate formulations using ultra-high performance liquid chromatography and triple quadrupole mass spectrometry

    Science.gov (United States)

    Tush, Daniel; Loftin, Keith A.; Meyer, Michael T.

    2013-01-01

    Little is known about the occurrence, fate, and effects of the ancillary additives in pesticide formulations. Polyoxyethylene tallow amine (POEA) is a non-ionic surfactant used in many glyphosate formulations, a widely applied herbicide both in agricultural and urban environments. POEA has not been previously well characterized, but has been shown to be toxic to various aquatic organisms. Characterization of technical mixtures using ultra-high performance liquid chromatography (UHPLC) and mass spectrometry shows POEA is a complex combination of homologs of different aliphatic moieties and ranges of ethoxylate units. Tandem mass spectrometry experiments indicate that POEA homologs generate no product ions readily suitable for quantitative analysis due to poor sensitivity. A comparison of multiple high performance liquid chromatography (HPLC) and UHPLC analytical columns indicates that the stationary phase is more important in column selection than other parameters for the separation of POEA. Analysis of several agricultural and household glyphosate formulations confirms that POEA is a common ingredient but ethoxylate distributions among formulations vary.

  11. Nontarget analysis of polar contaminants in freshwater sediments influenced by pharmaceutical industry using ultra-high-pressure liquid chromatography-quadrupole time-of-flight mass spectrometry

    International Nuclear Information System (INIS)

    Terzic, Senka; Ahel, Marijan

    2011-01-01

    A comprehensive analytical procedure for a reliable identification of nontarget polar contaminants in aquatic sediments was developed, based on the application of ultra-high-pressure liquid chromatography (UHPLC) coupled to hybrid quadrupole time-of-flight mass spectrometry (QTOFMS). The procedure was applied for the analysis of freshwater sediment that was highly impacted by wastewater discharges from the pharmaceutical industry. A number of different contaminants were successfully identified owing to the high mass accuracy of the QTOFMS system, used in combination with high chromatographic resolution of UHPLC. The major compounds, identified in investigated sediment, included a series of polypropylene glycols (n = 3-16), alkylbenzene sulfonate and benzalkonium surfactants as well as a number of various pharmaceuticals (chlorthalidone, warfarin, terbinafine, torsemide, zolpidem and macrolide antibiotics). The particular advantage of the applied technique is its capability to detect less known pharmaceutical intermediates and/or transformation products, which have not been previously reported in freshwater sediments. - Research highlights: → UHPLC-QTOFMS coupling was applied for nontarget analysis of polar contaminants. → Wide spectrum of polar contaminants was identified in polluted sediments. → Pharmaceuticals and their intermediates were present in high concentrations. - Comprehensive analysis of freshwater sediments by UPLC/QTOF indicated importance of pharmaceutically-derived polar contaminants.

  12. Nontarget analysis of polar contaminants in freshwater sediments influenced by pharmaceutical industry using ultra-high-pressure liquid chromatography-quadrupole time-of-flight mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Terzic, Senka, E-mail: terzic@irb.h [Division of Marine and Environmental Research, Rudjer Boskovic Institute, 10000 Zagreb (Croatia); Ahel, Marijan [Division of Marine and Environmental Research, Rudjer Boskovic Institute, 10000 Zagreb (Croatia)

    2011-02-15

    A comprehensive analytical procedure for a reliable identification of nontarget polar contaminants in aquatic sediments was developed, based on the application of ultra-high-pressure liquid chromatography (UHPLC) coupled to hybrid quadrupole time-of-flight mass spectrometry (QTOFMS). The procedure was applied for the analysis of freshwater sediment that was highly impacted by wastewater discharges from the pharmaceutical industry. A number of different contaminants were successfully identified owing to the high mass accuracy of the QTOFMS system, used in combination with high chromatographic resolution of UHPLC. The major compounds, identified in investigated sediment, included a series of polypropylene glycols (n = 3-16), alkylbenzene sulfonate and benzalkonium surfactants as well as a number of various pharmaceuticals (chlorthalidone, warfarin, terbinafine, torsemide, zolpidem and macrolide antibiotics). The particular advantage of the applied technique is its capability to detect less known pharmaceutical intermediates and/or transformation products, which have not been previously reported in freshwater sediments. - Research highlights: UHPLC-QTOFMS coupling was applied for nontarget analysis of polar contaminants. Wide spectrum of polar contaminants was identified in polluted sediments. Pharmaceuticals and their intermediates were present in high concentrations. - Comprehensive analysis of freshwater sediments by UPLC/QTOF indicated importance of pharmaceutically-derived polar contaminants.

  13. Distribution patterns of flavonoids from three Momordica species by ultra-high performance liquid chromatography quadrupole time of flight mass spectrometry: a metabolomic profiling approach

    Directory of Open Access Journals (Sweden)

    Ntakadzeni Edwin Madala

    Full Text Available ABSTRACT Plants from the Momordica genus, Curcubitaceae, are used for several purposes, especially for their nutritional and medicinal properties. Commonly known as bitter gourds, melon and cucumber, these plants are characterized by a bitter taste owing to the large content of cucurbitacin compounds. However, several reports have shown an undisputed correlation between the therapeutic activities and polyphenolic flavonoid content. Using ultra-high performance liquid chromatography quadrupole time of flight mass spectrometry in combination with multivariate data models such as principal component analysis and hierarchical cluster analysis, three Momordica species (M. foetida Schumach., M. charantia L. and M. balsamina L. were chemo-taxonomically grouped based on their flavonoid content. Using a conventional mass spectrometric-based approach, thirteen flavonoids were tentatively identified and the three species were found to contain different isomers of the quercetin-, kaempferol- and isorhamnetin-O-glycosides. Our results indicate that Momordica species are overall very rich sources of flavonoids but do contain different forms thereof. Furthermore, to the best of our knowledge, this is a first report on the flavonoid content of M. balsamina L.

  14. Multicomponent mixed dopant optimization for rapid screening of polycyclic aromatic hydrocarbons using ultra high performance liquid chromatography coupled to atmospheric pressure photoionization high-resolution mass spectrometry

    KAUST Repository

    Sioud, Salim

    2012-05-04

    RATIONALE To enhance the ionization efficiencies in atmospheric pressure photoionization mass spectrometry a dopant with favorable ionization energy such as chlorobenzene is typically used. These dopants are typically toxic and difficult to mix with water-soluble organic solvents. In order to achieve a more efficient and less toxic dopant, a multicomponent mixed dopant was explored. METHODS A multicomponent mixed dopant for non-targeted rapid screening of polycyclic aromatic hydrocarbons (PAHs) was developed and optimized using ultra high performance liquid chromatography (UPLC) coupled to atmospheric pressure photoionization high-resolution mass spectrometry. Various single and multicomponent mixed dopants consisting of ethanol, chlorobenzene, bromobenzene, anisole and toluene were evaluated. RESULTS Fourteen out of eighteen PAHs were successfully separated and detected at low pg/μL levels within 5 min with high mass accuracy ≤4 ppm. The optimal mixed multicomponent dopant consisted of ethanol/chlorobenzene/bromobenzene/anisole (98.975:0.1:0.9:0.025, v/v %) and it improved the limit of detection (LOD) by 2- to 10-fold for the tested PAHs compared to those obtained with pure chlorobenzene. CONCLUSIONS A novel multicomponent dopant that contains 99% ethanol and 1% mixture of chlorobenzene, bromobenzene and anisole was found to be an effective dopant mixture to ionize PAHs. The developed UPLC multicomponent dopant assisted atmospheric pressure photoionization high-resolution mass spectrometry offered a rapid non targeted screening method for detecting the PAHs at low pg/;μL levels within a 5 min run time with high mass accuracy a;circ4 ppm. Copyright © 2012 John Wiley & Sons, Ltd.

  15. The Evolution of MALDI-TOF Mass Spectrometry toward Ultra-High-Throughput Screening: 1536-Well Format and Beyond.

    Science.gov (United States)

    Haslam, Carl; Hellicar, John; Dunn, Adrian; Fuetterer, Arne; Hardy, Neil; Marshall, Peter; Paape, Rainer; Pemberton, Michelle; Resemannand, Anja; Leveridge, Melanie

    2016-02-01

    Mass spectrometry (MS) offers a label-free, direct-detection method, in contrast to fluorescent or colorimetric methodologies. Over recent years, solid-phase extraction-based techniques, such as the Agilent RapidFire system, have emerged that are capable of analyzing samples in high-throughput screening (HTS). Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF) offers an alternative for high-throughput MS detection. However, sample preparation and deposition onto the MALDI target, as well as interference from matrix ions, have been considered limitations for the use of MALDI for screening assays. Here we describe the development and validation of assays for both small-molecule and peptide analytes using MALDI-TOF coupled with nanoliter liquid handling. Using the JMJD2c histone demethylase and acetylcholinesterase as model systems, we have generated robust data in a 1536 format and also increased sample deposition to 6144 samples per target. Using these methods, we demonstrate that this technology can deliver fast sample analysis time with low sample volume, and data comparable to that of current RapidFire assays. © 2015 Society for Laboratory Automation and Screening.

  16. Indirect enantioseparation of fluoxetine in mouse serum by derivatization with 1R-(-)-menthyl chloroformate followed by ultra high performance liquid chromatography and quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Zhao, Jing; Jin, Yan; Shin, Yujin; Jeong, Kyung Min; Lee, Jeongmi

    2016-03-01

    Here we describe a simple and sensitive analytical method for the enantioselective quantification of fluoxetine in mouse serum using ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry. The sample preparation method included a simple deproteinization with acetonitrile in 50 μL of serum, followed by derivatization of the extracts in 50 μL of 2 mM 1R-(-)-menthyl chloroformate at 45ºC for 55 min. These conditions were statistically optimized through response surface methodology using a central composite design. Under the optimized conditions, neither racemization nor kinetic resolution occurred. The derivatized diastereomers were readily resolved on a conventional sub-2 μm C18 column under a simple gradient elution of aqueous methanol containing 0.1% formic acid. The established method was validated and found to be linear, precise, and accurate over the concentration range of 5.0-1000.0 ng/mL for both R and S enantiomers (r(2) > 0.993). Stability tests of the prepared samples at three different concentration levels showed that the R- and S-fluoxetine derivatives were relatively stable for 48 h. No significant matrix effects were observed. Last, the developed method was successfully used for enantiomeric analysis of real serum samples collected at a number of time points from mice administered with racemic fluoxetine. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Countercurrent chromatography separation of saponins by skeleton type from Ampelozizyphus amazonicus for off-line ultra-high-performance liquid chromatography/high resolution accurate mass spectrometry analysis and characterisation.

    Science.gov (United States)

    de Souza Figueiredo, Fabiana; Celano, Rita; de Sousa Silva, Danila; das Neves Costa, Fernanda; Hewitson, Peter; Ignatova, Svetlana; Piccinelli, Anna Lisa; Rastrelli, Luca; Guimarães Leitão, Suzana; Guimarães Leitão, Gilda

    2017-01-20

    Ampelozizyphus amazonicus Ducke (Rhamnaceae), a medicinal plant used to prevent malaria, is a climbing shrub, native to the Amazonian region, with jujubogenin glycoside saponins as main compounds. The crude extract of this plant is too complex for any kind of structural identification, and HPLC separation was not sufficient to resolve this issue. Therefore, the aim of this work was to obtain saponin enriched fractions from the bark ethanol extract by countercurrent chromatography (CCC) for further isolation and identification/characterisation of the major saponins by HPLC and MS. The butanol extract was fractionated by CCC with hexane - ethyl acetate - butanol - ethanol - water (1:6:1:1:6; v/v) solvent system yielding 4 group fractions. The collected fractions were analysed by UHPLC-HRMS (ultra-high-performance liquid chromatography/high resolution accurate mass spectrometry) and MS n . Group 1 presented mainly oleane type saponins, and group 3 showed mainly jujubogenin glycosides, keto-dammarane type triterpene saponins and saponins with C 31 skeleton. Thus, CCC separated saponins from the butanol-rich extract by skeleton type. A further purification of group 3 by CCC (ethyl acetate - ethanol - water (1:0.2:1; v/v)) and HPLC-RI was performed in order to obtain these unusual aglycones in pure form. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Quantification of 15 bile acids in lake charr feces by ultra-high performance liquid chromatography–tandem mass spectrometry

    Science.gov (United States)

    Li, Ke; Buchinger, Tyler J.; Bussy, Ugo; Fissette, Skye D.; Johnson, Nicholas; Li, Weiming

    2015-01-01

    Many fishes are hypothesized to use bile acids (BAs) as chemical cues, yet quantification of BAs in biological samples and the required methods remain limited. Here, we present an UHPLC–MS/MS method for simultaneous, sensitive, and rapid quantification of 15 BAs, including free, taurine, and glycine conjugated BAs, and application of the method to fecal samples from lake charr (Salvelinus namaycush). The analytes were separated on a C18 column with acetonitrile–water (containing 7.5 mM ammonium acetate and 0.1% formic acid) as mobile phase at a flow rate of 0.25 mL/min for 12 min. BAs were monitored with a negative electrospray triple quadrupole mass spectrometer (Xevo TQ-S™). Calibration curves of 15 BAs were linear over the concentration range of 1.00–5,000 ng/mL. Validation revealed that the method was specific, accurate, and precise. The method was applied to quantitative analysis of feces extract of fry lake charr and the food they were eating. The concentrations of analytes CA, TCDCA, TCA, and CDCA were 242.3, 81.2, 60.7, and 36.2 ng/mg, respectively. However, other taurine conjugated BAs, TUDCA, TDCA, and THDCA, were not detected in feces of lake charr. Interestingly, TCA and TCDCA were detected at high concentrations in food pellets, at 71.9 and 38.2 ng/mg, respectively. Application of the method to feces samples from lake charr supported a role of BAs as chemical cues, and will enhance further investigation of BAs as chemical cues in other fish species.

  19. Quantification of Oxidized and Unsaturated Bile Alcohols in Sea Lamprey Tissues by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Ke Li

    2016-08-01

    Full Text Available A sensitive and reliable method was developed and validated for the determination of unsaturated bile alcohols in sea lamprey tissues using liquid-liquid extraction and ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS. The liver, kidney, and intestine samples were extracted with acetonitrile and defatted by n-hexane. Gradient UHPLC separation was performed using an Acquity BEH C18 column with a mobile phase of water and methanol containing 20 mM triethylamine. Multiple reaction monitoring modes of precursor-product ion transitions for each analyte was used. This method displayed good linearity, with correlation coefficients greater than 0.99, and was validated. Precision and accuracy (RSD % were in the range of 0.31%–5.28%, while mean recoveries were between 84.3%–96.3%. With this technique, sea lamprey tissue samples were analyzed for unsaturated bile alcohol analytes. This method is practical and particularly suitable for widespread putative pheromone residue analysis.

  20. Analysis of new psychoactive substances in oral fluids by means of microextraction by packed sorbent followed by ultra-high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Rocchi, Rachele; Simeoni, Maria Chiara; Montesano, Camilla; Vannutelli, Gabriele; Curini, Roberta; Sergi, Manuel; Compagnone, Dario

    2017-10-27

    In recent years, new drugs, commonly known as new psychoactive substances (NPS), appeared on the market, which include, among others, synthetic cannabinoids, cathinones, and tryptamine analogs of psilocin. The aim of this work was to develop and validate a new method for simultaneous screening and quantification of 31 NPS in oral fluid by ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The chosen target analytes represented different chemical and toxicological NPS classes, such as synthetic cathinones, piperazines, phenethylamines, synthetic cannabinoids, and their metabolites. The procedure involved a rapid sample preparation based on protein precipitation followed by clean-up utilizing microextraction by packed sorbent (MEPS); the quantitative analysis was performed by UHPLC-MS/MS. The MEPS clean-up, regardless of non-quantitative recoveries for some analytes, provided an effective removal of interfering compounds, as demonstrated by reduced matrix effects found at different concentrations for all the analytes. The validation protocol, based on SWGTOX guidelines, demonstrated the suitability of the proposed method for quantitative analysis: linearity range ranged over 3 or 4 orders of magnitude; precision and accuracy tests gave RSD% values below 25%, and accuracy ranged from 85.9% to 107%, accomplishing SWGTOX requirements. Limits of detection (LODs) ranged between 0.005 ng/mL and 0.850 ng/mL and limits of quantification (LOQs) from 0.015 to 2.600 ng/mL. Copyright © 2017 John Wiley & Sons, Ltd.

  1. A high-throughput screening method of bisphenols, bisphenols digycidyl ethers and their derivatives in dairy products by ultra-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Cheng, Yan; Nie, Xue-Mei; Wu, Han-Qiu; Hong, Yun-He; Yang, Bing-Cheng; Liu, Tong; Zhao, Dan; Wang, Jian-Feng; Yao, Gui-Hong; Zhang, Feng

    2017-01-15

    A simple and universal analytical method based on ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for high throughput screening of 21 bisphenols, bisphenols digycidyl ethers and their derivatives in dairy products was developed. Response Surface Methodology (RSM) was used to optimize sample preparation conditions based on a quick, easy, cheap, effective, rugged and safe (QuEChERS) method. The analytes were extracted by using 15 mL acetonitrile with 1% acetic acid, and the extracts were further purified by using 190 mg of C18 and 390 mg of PSA. The extracts were analyzed by UHPLC-MS/MS with electrospray ionization (ESI) source. Linearity was assessed by using matrix-matched standard calibration and good correlation coefficients (r 2  > 0.99) were obtained. The limits of quantitation (LOQs) for the analytes ranged from 0.02 to 5 μg kg -1 . The extraction recoveries were in a range of 88.2%-108.2%. Good method reproducibility in terms of intra- and inter-day precision was observed, yielding relative standard deviations (RSDs) less than 8.9% and 9.9%, respectively. The validation method results revealed that the proposed method was sensitive and reliable. Finally, this method was successfully applied to dairy product analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Advances in ultra-high performance liquid chromatography coupled to tandem mass spectrometry for sensitive detection of several food allergens in complex and processed foodstuffs.

    Science.gov (United States)

    Planque, M; Arnould, T; Dieu, M; Delahaut, P; Renard, P; Gillard, N

    2016-09-16

    Sensitive detection of food allergens is affected by food processing and foodstuff complexity. It is therefore a challenge to detect cross-contamination in food production that could endanger an allergic customer's life. Here we used ultra-high performance liquid chromatography coupled to tandem mass spectrometry for simultaneous detection of traces of milk (casein, whey protein), egg (yolk, white), soybean, and peanut allergens in different complex and/or heat-processed foodstuffs. The method is based on a single protocol (extraction, trypsin digestion, and purification) applicable to the different tested foodstuffs: chocolate, ice cream, tomato sauce, and processed cookies. The determined limits of quantitation, expressed in total milk, egg, peanut, or soy proteins (and not soluble proteins) per kilogram of food, are: 0.5mg/kg for milk (detection of caseins), 5mg/kg for milk (detection of whey), 2.5mg/kg for peanut, 5mg/kg for soy, 3.4mg/kg for egg (detection of egg white), and 30.8mg/kg for egg (detection of egg yolk). The main advantage is the ability of the method to detect four major food allergens simultaneously in processed and complex matrices with very high sensitivity and specificity. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Determination of anthelmintic drug residues in milk using ultra high performance liquid chromatography-tandem mass spectrometry with rapid polarity switching.

    Science.gov (United States)

    Whelan, Michelle; Kinsella, Brian; Furey, Ambrose; Moloney, Mary; Cantwell, Helen; Lehotay, Steven J; Danaher, Martin

    2010-07-02

    A new UHPLC-MS/MS (ultra high performance liquid chromatography coupled to tandem mass spectrometry) method was developed and validated to detect 38 anthelmintic drug residues, consisting of benzimidazoles, avermectins and flukicides. A modified QuEChERS-type extraction method was developed with an added concentration step to detect most of the analytes at keeper to ensure analytes remain in solution. Using rapid polarity switching in electrospray ionisation, a single injection was capable of detecting both positively and negatively charged ions in a 13 min run time. The method was validated at two levels: the unapproved use level and at the maximum residue level (MRL) according to Commission Decision (CD) 2002/657/EC criteria. The decision limit (CCalpha) of the method was in the range of 0.14-1.9 and 11-123 microg kg(-1) for drugs validated at unapproved and MRL levels, respectively. The performance of the method was successfully verified for benzimidazoles and levamisole by participating in a proficiency study.

  4. Development of a Novel, Sensitive, Selective, and Fast Methodology to Determine Malondialdehyde in Leaves of Melon Plants by Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Melisa E. Yonny

    2017-01-01

    Full Text Available Early production of melon plant (Cucumis melo is carried out using tunnels structures, where extreme temperatures lead to high reactive oxygen species production and, hence, oxidative stress. Malondialdehyde (MDA is a recognized biomarker of the advanced oxidative status in a biological system. Thus a reliable, sensitive, simple, selective, and rapid separative strategy based on ultra-high-performance liquid chromatography coupled to positive electrospray-tandem mass spectrometry (UPLC-(+ESI-MS/MS was developed for the first time to measure MDA, without derivatization, in leaves of melon plants exposed to stress conditions. The detection and quantitation limits were 0.02 μg·L−1 and 0.08 μg·L−1, respectively, which was demonstrated to be better than the methodologies currently reported in the literature. The accuracy values were between 96% and 104%. The precision intraday and interday values were 2.7% and 3.8%, respectively. The optimized methodology was applied to monitoring of changes in MDA levels between control and exposed to thermal stress conditions melon leaves samples. Important preliminary conclusions were obtained. Besides, a comparison between MDA levels in melon leaves quantified by the proposed method and the traditional thiobarbituric acid reactive species (TBARS approach was undertaken. The MDA determination by TBARS could lead to unrealistic conclusions regarding the oxidative stress status in plants.

  5. Simultaneous Determination of Fifteen Constituents of Jitai Tablet Using Ultra High-Performance Liquid Chromatography Coupled with Triple Quadrupole Electrospray Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Shuping Wang

    2014-01-01

    Full Text Available An ultra-high-performance liquid chromatography-electrospray ionization tandem mass spectrometry (UHPLC-ESI-MS/MS method was developed for simultaneous determination of fifteen constituents in Jitai tablet (JTT, a complex Traditional Chinese Medicine prescription (TCMP used in treating opiate addiction. Benefitting from a small particle size (1.8 µm C18 column, accelerated analysis with satisfactory resolution, sensitivity and selectivity were achieved in a single run within 7 min with linear gradient elution of acetonitrile-0.1% (v/v formic acid in water. The analytical signal was obtained by multiple reaction monitoring transitions via electrospray ionization source operating in both positive and negative ionization mode. The approach was validated for linearity, sensitivity, precision, repeatability, stability and recovery. All analytes showed good linearity over a wide concentration range (r > 0.99. The method limits ranged from 0.03 ng/mL to 19.35 ng/mL which are sensitive enough for quality control studies. The developed method was successfully applied to the simultaneous determination of fifteen constituents in JTT. In conclusion, our experimental results demonstrate that UHPLC-ESI-MS/MS is a useful approach for the overall quality assessment of complex TCMPs.

  6. Fast analysis of 29 polycyclic aromatic hydrocarbons (PAHs) and nitro-PAHs with ultra-high performance liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry

    Science.gov (United States)

    Lung, Shih-Chun Candice; Liu, Chun-Hu

    2015-01-01

    Polycyclic aromatic hydrocarbons (PAHs) and nitro-PAHs are ubiquitous in the environment. Some of them are probable carcinogens and some are source markers. This work presents an ultra-high performance liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry (UHPLC-APPI-MS/MS) method for simultaneous analysis of 20 PAHs and nine nitro-PAHs. These compounds are separated in 15 minutes in the positive mode and 11 minutes in the negative mode, one half of GC/MS analysis time. Two pairs of precursor/product ions are offered, which is essential for confirmation. This method separates and quantifies benzo[a]pyrene (the most toxic PAHs) and non-priority benzo[e]pyrene (isomers, little toxicity) to avoid overestimation of toxin levels, demonstrating its importance for health-related researches. With 0.5% 2,4-difluoroanisole in chlorobenzene as the dopant, limits of detection of PAHs except acenaphthylene and those of nitro-PAHs except 2-nitrofluoranthene are below 10 pg and 3 pg, respectively, mostly lower than or comparable to those reported using LC-related systems. The responses were linear over two orders of magnitude with fairly good accuracy and precision. Certified reference materials and real aerosol samples were analyzed to demonstrate its applicability. This fast, sensitive, and reliable method is the first UHPLC-APPI-MS/MS method capable of simultaneously analyzing 29 environmentally and toxicologically important PAHs and nitro-PAHs. PMID:26265155

  7. Ultra high performance liquid chromatography-electrospray ionization-tandem mass spectrometry screening method for direct analysis of designer drugs, "spice" and stimulants in oral fluid.

    Science.gov (United States)

    Strano-Rossi, Sabina; Anzillotti, Luca; Castrignanò, Erika; Romolo, Francesco Saverio; Chiarotti, Marcello

    2012-10-05

    An ultra high performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UHPLC-ESI-MS/MS) screening method for the direct analysis in oral fluid (OF) of 24 drugs, including new synthetic cannabinoids and so-called "smart" designer drugs, in a single chromatographic run was set up. Benzylpiperazine, methylone, 5,6-methylenedioxy-2-aminoindane (MDAI), fenproporex, 4-fluoroamphetamine (4-FA), 4-methyl-N-ethylcathinone (4-MEC), 4-methylamphetamine (4-MA), methylbenzodioxolylbutanamine (MBDB), mephedrone, methylthioamphetamine (MTA), methylenedioxypyrovalerone (MDPV), mefenorex, nabilone, furfenorex, clobenzorex, JWH-200, AM 694, JWH-250, JWH-073, JWH-018, JWH-019, JWH-122, HU 210 and CP 47497 were determined in a chromatographic run of 9 min only with no sample pre-treatment, after addition of ISs and dilution in mobile phase A. This method is designed to be applied to 250 μL of OF sample, anyway is suitable to be used on smaller volumes (till 100 μL). LODs vary from 1ng/mL to 20 ng/mL. No interfering peaks were observed due to similar analytes, common therapeutic drugs or endogenous compounds. Matrix effect, although present especially for mephedrone, is acceptable, allowing the detection of the compounds at the LODs described. The developed method was applied on 400 real OF samples from on-site tests performed by police officers. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. An isotope dilution ultra high performance liquid chromatography-tandem mass spectrometry method for the simultaneous determination of sugars and humectants in tobacco products.

    Science.gov (United States)

    Wang, Liqun; Cardenas, Roberto Bravo; Watson, Clifford

    2017-09-08

    CDC's Division of Laboratory Sciences developed and validated a new method for the simultaneous detection and measurement of 11 sugars, alditols and humectants in tobacco products. The method uses isotope dilution ultra high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS) and has demonstrated high sensitivity, selectivity, throughput and accuracy, with recoveries ranging from 90% to 113%, limits of detection ranging from 0.0002 to 0.0045μg/mL and coefficients of variation (CV%) ranging from 1.4 to 14%. Calibration curves for all analytes were linear with linearity R 2 values greater than 0.995. Quantification of tobacco components is necessary to characterize tobacco product components and their potential effects on consumer appeal, smoke chemistry and toxicology, and to potentially help distinguish tobacco product categories. The researchers analyzed a variety of tobacco products (e.g., cigarettes, little cigars, cigarillos) using the new method and documented differences in the abundance of selected analytes among product categories. Specifically, differences were detected in levels of selected sugars found in little cigars and cigarettes, which could help address appeal potential and have utility when product category is unknown, unclear, or miscategorized. Copyright © 2017. Published by Elsevier B.V.

  9. Ultra-high-performance liquid chromatography-tandem mass spectrometry measurement of climbazole deposition from hair care products onto artificial skin and human scalp.

    Science.gov (United States)

    Chen, Guoqiang; Hoptroff, Michael; Fei, Xiaoqing; Su, Ya; Janssen, Hans-Gerd

    2013-11-22

    A sensitive and specific ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated for the measurement of climbazole deposition from hair care products onto artificial skin and human scalp. Deuterated climbazole was used as the internal standard. Atmospheric pressure chemical ionization (APCI) in positive mode was applied for the detection of climbazole. For quantification, multiple reaction monitoring (MRM) transition 293.0>69.0 was monitored for climbazole, and MRM transition 296.0>225.1 for the deuterated climbazole. The linear range ran from 4 to 2000 ng mL(-1). The limit of detection (LOD) and the limit of quantification (LOQ) were 1 ng mL(-1) and 4 ng mL(-1), respectively, which enabled quantification of climbazole on artificial skin and human scalp at ppb level (corresponding to 16 ng cm(-2)). For the sampling of climbazole from human scalp the buffer scrub method using a surfactant-modified phosphate buffered saline (PBS) solution was selected based on a performance comparison of tape stripping, the buffer scrub method and solvent extraction in in vitro studies. Using this method, climbazole deposition in in vitro and in vivo studies was successfully quantified. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. A Method for Multiple Mycotoxin Analysis in Wines by Solid Phase Extraction and Multifunctional Cartridge Purification, and Ultra-High-Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry

    Science.gov (United States)

    Tamura, Masayoshi; Takahashi, Ayumi; Uyama, Atsuo; Mochizuki, Naoki

    2012-01-01

    An analytical method using two solid phase extractions and ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) was developed for the identification and quantification of 14 mycotoxins (patulin, deoxynivalenol, aflatoxins B1, B2, G1, G2, M1, T-2 toxin, HT-2 toxin, zearalenone, fumonisins B1, B2, B3, and ochratoxin A) in domestic and imported wines. Mycotoxins were purified with an Oasis HLB cartridge, followed by a MultiSepTM #229 Ochra. As a result, sufficient removal of the pigments and highly polar matrices from the red wines was achieved. UHPLC conditions were optimized, and 14 mycotoxins were separated in a total of 13 min. Determinations performed using this method produced high correlation coefficients for the 14 mycotoxins (R > 0.990) and recovery rates ranging from 76 to 105% with good repeatability (relative standard deviation RSD < 12%). Twenty-seven samples of domestic and imported wines were analyzed using this method. Although ochratoxin A (OTA) and fumonisins (FMs) were detected in several samples, the FM levels were less than limits of quantification (LOQs) (1 μg/L), and even the largest of the OTA levels was below the EU regulatory level (2 μg/L). These results suggest that the health risk posed to consumers from the wines available in Japan is relatively low. PMID:22822458

  11. Determination of steroid hormones in fish tissues by microwave-assisted extraction coupled to ultra-high performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Guedes-Alonso, Rayco; Sosa-Ferrera, Zoraida; Santana-Rodríguez, José Juan

    2017-12-15

    Steroid hormones produce adverse effects on biota as well as bioaccumulation in fish and seafood, making it necessary to develop methodologies to evaluate these compounds in samples related to the food chain. This work presents an analytical method for evaluating 15 steroid hormones in fish tissue. It is based on microwave-assisted extraction and solid-phase extraction coupled to ultra-high-performance liquid chromatography tandem mass spectrometry (MAE-SPE-UHPLC-MS/MS). The proposed method shows appropriate detection limits (0.14-49.0ngg -1 ), recoveries in the range of 50% and good repeatability. After optimization, the method was applied to different tissues from two small fishes of the Canary Islands that constitute an important level of the food web (Boops boops and Sphoeroides marmoratus) and were exposed to the outfall of the Las Palmas de Gran Canaria wastewater treatment plant. The concentrations of eight detected compounds ranged from below the quantification limits to 3.95μgg -1 . Copyright © 2017 Elsevier Ltd. All rights reserved.

  12. Simultaneous quantitative determination of 11 sesquiterpene lactones in Jerusalem artichoke (Helianthus tuberosus L.) leaves by ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Yuan, Xiaoyan; Yang, Qianxu

    2017-04-01

    A method of ultra high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry was developed for the simultaneous quantification of 11 sesquiterpene lactones in 11 Jerusalem artichoke leaf samples harvested in a number of areas at different periods. The optimal chromatographic conditions were achieved on a ZORBAX Eclipse Plus C 18 column (3.0 × 150 mm, 1.8 μm) with linear gradient elution of methanol and water in 8 min. Quantitative analysis was carried out under selective ion monitoring mode. All of the sesquiterpene lactones showed good linearity (R 2 ≥ 0.9949), repeatability (relative standard deviations Jerusalem artichoke leaf samples from different areas. Among them, the content of sesquiterpene lactones in the sample collected from Dalian, Liaoning province was the highest and the early flowering period was considered to be the optimal harvest time. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Simultaneous determination of fumonisins B1, B2 and B3 contaminants in maize by ultra high-performance liquid chromatography tandem mass spectrometry

    International Nuclear Information System (INIS)

    Ren Yiping; Zhang Yu; Han Shiyun; Han Zheng; Wu Yongning

    2011-01-01

    The present work developed an analytical method for simultaneous determination of fumonisins B 1 , B 2 and B 3 residues in maize by ultra high-performance liquid chromatography combined with electrospray ionization triple quadrupole tandem mass spectrometry (UHPLC-MS/MS) under the multiple reaction monitoring (MRM) mode, and especially focused on the optimization of extraction, clean-up, UHPLC separation and MS/MS parameters. The method involves addition of fumonisins isotope internal standards, extraction with a mixture of acetonitrile and water and clean-up with solid-phase extraction (SPE) cartridges before UHPLC-MS/MS analysis. A single-laboratory method validation was conducted by testing three different spiking levels for repeatability and recovery according to International Union of Pure and Applied Chemistry (IUPAC) guidelines. The LOQ of FB 1 , FB 2 and FB 3 were 1.50, 1.65 and 0.4 μg kg -1 , respectively, which were lower than the criteria of EU, USA and other countries regarding minimum residue limits of fumonisins in foods including baby foods and feedstuffs. Recoveries of three fumonisins ranged from 80.9% to 97.0% with RSD values of 2.4-11.1%.The advantages of this method include simple pretreatment, rapid determination and high sensitivity, and it fulfills the requirements for food analysis with respect to minimum residue limits of fumonisins in various countries.

  14. Characterization of the multiple components of Acanthopanax Senticosus stem by ultra high performance liquid chromatography with quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Sun, Hui; Liu, Jianhua; Zhang, Aihua; Zhang, Ying; Meng, Xiangcai; Han, Ying; Zhang, Yingzhi; Wang, Xijun

    2016-02-01

    Acanthopanax Senticosus Harms. has been used widely in traditional Chinese medicine for the treatment of chronic bronchitis, neurasthenia, hypertension and ischemic heart disease. However, the in vivo constituents of the stem of Acanthopanax Senticosus remain unknown. In this paper, ultra high performance liquid chromatography with electrospray ionization quadrupole time-of-flight mass spectrometry and the MarkerLynx(TM) software combined with multiple data processing approach were used to study the constituents in vitro and in vivo. The aqueous extract from the Acanthopanax Senticosus stem and the compositions in rat serum after intragastric administration were completely analyzed. Consequently, 115 compounds in the aqueous extract from Acanthopanax Senticosus stem and 41 compounds absorbed into blood were characterized. Of the 115 compounds in vitro, 54 were reported for first time, including sinapyl alcohol, sinapyl alcohol diglucoside, and 1-O-sinapoyl-β-D-glucose. In the 41 compounds in vivo, 7 were prototype components and 34 were metabolites which were from 21 components of aqueous extract from Acanthopanax Senticosus stem, and the metabolic pathways of the metabolites were elucidated for first time. The results narrowed the range of screening the active components and provided a basis for the study of action mechanism and pharmacology. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Metabolic profiles of physalin A in rats using ultra-high performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Feng, Xinchi; Liu, Hongxia; Chai, Liwei; Ding, Liqin; Pan, Guixiang; Qiu, Feng

    2017-03-01

    Physalin A, one of the major active components isolated from the calyces of Physalis alkekengi var. franchetii is considered to be a promising natural product due to its anti-inflammatory and excellent antitumor activities. Until now, only one paper is available from our group concerning identification of two sulfonate metabolites from rat feces after physalin A treatment. All the other researches related to physalin A were focused on its extraction, separation and biological activities. In this research, a rapid and reliable ultra-high-performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UPLC/Q-TOF-MS/MS) method was developed and employed for the comprehensive study of the metabolism of physalin A in vivo for the first time. A total of 24 proposed metabolites were identified in plasma, bile, urine and feces of rats after oral administration of physalin A. The results indicated that sulfonation, reduction and hydroxylation were the major metabolic pathways of physalin A in vivo. Furthermore, this research provides scientific and reliable support for full understanding of the metabolism of physalin A and the results could help to elucidate the safety and efficacy of physalin A, as well as other physalins. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Ultra-high performance liquid chromatography tandem mass spectrometry for the determination of five glycopeptide antibiotics in food and biological samples using solid-phase extraction.

    Science.gov (United States)

    Deng, Fenfang; Yu, Hong; Pan, Xinhong; Hu, Guoyuan; Wang, Qiqin; Peng, Rongfei; Tan, Lei; Yang, Zhicong

    2018-02-23

    This paper demonstrated the development and validation of an ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method for simultaneous determination of five glycopeptide antibiotics in food and biological samples. The target glycopeptide antibiotics were isolated from the samples by solvent extraction, and the extracts were cleaned with a tandem solid-phase extraction step using mixed strong cation exchange and hydrophilic/lipophilic balance cartridges. Subsequently, the analytes were eluted with different solvents, and then quantified by UHPLC-MS/MS in the positive ionization mode with multiple reaction monitoring. Under optimal conditions, good linear correlations were obtained for the five glycopeptide antibiotics in the concentration range of 1.0 μg/L to 20.0 μg/L, and with linear correlation coefficients >0.998. Employing this method, the target glycopeptide antibiotics in food and biological samples were identified with a recovery of 83.0-102%, and a low quantitation limit of 1.0 μg/kg in food and 2.0 μg/L in biological samples with low matrix effects. Copyright © 2018 Elsevier B.V. All rights reserved.

  17. Hydrophilic interaction ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometry for determination of nucleotides, nucleosides and nucleobases in Ziziphus plants.

    Science.gov (United States)

    Guo, Sheng; Duan, Jin-ao; Qian, Dawei; Wang, Hanqing; Tang, Yuping; Qian, Yefei; Wu, Dawei; Su, Shulan; Shang, Erxin

    2013-08-02

    In this study, a rapid and sensitive analytical method was developed for the determination of 20 nucleobases, nucleosides and nucleotides in Ziziphus plants at trace levels by using hydrophilic interaction ultra-high performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (HILIC-UHPLC-TQ-MS/MS) in multiple-reaction monitoring (MRM) mode. Under the optimized chromatographic conditions, good separation for 20 target compounds were obtained on a UHPLC Amide column with sub-2μm particles within 10min. The overall LODs and LOQs were between 0.11-3.12ngmL(-1) and 0.29-12.48ngmL(-1) for the 20 analytes, respectively. It is the first report about simultaneous analysis of nucleobases, nucleosides and nucleotides in medicinal plants using HILIC-UHPLC-TQ-MS/MS method, which affords good linearity, precision, repeatability and accuracy. The developed method was successfully applied to Ziziphus plant (Z. jujuba, Z. jujuba var. spinosa and Z. mauritiana) samples. The analysis showed that the fruits and leaves of Ziziphus plants are rich in nucleosides and nucleobases as well as nucleotides, and could be selected as the healthy food resources. Our results in present study suggest that HILIC-UHPLC-TQ-MS/MS method could be employed as a useful tool for quality assessment of the samples from the Ziziphus plants as well as other medicinal plants or food samples using nucleotides, nucleosides and nucleobases as markers. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Multi-target determination of organic ultraviolet absorbents in organism tissues by ultrasonic assisted extraction and ultra-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Peng, Xianzhi; Jin, Jiabin; Wang, Chunwei; Ou, Weihui; Tang, Caiming

    2015-03-06

    A sensitive and reliable method was developed for multi-target determination of 13 most widely used organic ultraviolet (UV) absorbents (including UV filters and UV stabilizers) in aquatic organism tissues. The organic UV absorbents were extracted using ultrasonic-assisted extraction, purified via gel permeation chromatography coupled with silica gel column chromatography, and determined by ultra-high performance liquid chromatography-tandem mass spectrometry. Recoveries of the UV absorbents from organism tissues mostly ranged from 70% to 120% from fish filet with satisfactory reproducibility. Method quantification limits were 0.003-1.0ngg(-1) dry weight (dw) except for 2-ethylhexyl 4-methoxycinnamate. This method has been applied to analysis of the UV absorbents in wild and farmed aquatic organisms collected from the Pearl River Estuary, South China. 2-Hydroxy-4-methoxybenzophenone and UV-P were frequently detected in both wild and farmed marine organisms at low ngg(-1)dw. 3-(4-Methylbenzylidene)camphor and most of the benzotriazole UV stabilizers were also frequently detected in maricultured fish. Octocrylene and 2-ethylhexyl 4-methoxycinnamate were not detected in any sample. This work lays basis for in-depth study about bioaccumulation and biomagnification of the UV absorbents in marine environment. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Ultra-high performance liquid chromatography coupled to mass spectrometry applied to the identification of valuable phenolic compounds from Eucalyptus wood.

    Science.gov (United States)

    Santos, Sónia A O; Vilela, Carla; Freire, Carmen S R; Neto, Carlos Pascoal; Silvestre, Armando J D

    2013-11-01

    Ultra-high performance liquid chromatography (UHPLC) was applied for the first time in the analysis of wood extracts. The potential of this technique coupled to ion trap mass spectrometry in the rapid and effective detection and identification of bioactive components in complex vegetal samples was demonstrated. Several dozens of compounds were detected in less than 30min of analysis time, corresponding to more than 3-fold reduction in time, when compared to conventional HPLC analysis of similar extracts. The phenolic chemical composition of Eucalyptus grandis, Eucalyptus urograndis (E. grandis×E. urophylla) and Eucalyptus maidenii wood extracts was assessed for the first time, with the identification of 51 phenolic compounds in the three wood extracts. Twenty of these compounds are reported for the first time as Eucalyptus genus components. Ellagic acid and ellagic acid-pentoside are the major components in all extracts, followed by gallic and quinic acids in E. grandis and E. urograndis and ellagic acid-pentoside isomer, isorhamnetin-hexoside and gallic acid in E. maidenii. The antioxidant scavenging activity of the extracts was evaluated, with E. grandis wood extract showing the lowest IC50 value. Moreover, the antioxidant activity of these extracts was higher than that of the commercial antioxidant BHT and of those of the corresponding bark extracts. These results, together with the phenolic content values, open good perspectives for the exploitation of these renewable resources as a source of valuable phenolic compounds. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Ultra-high-performance liquid chromatography tandem mass spectrometry method for the determination of gambogenic acid in dog plasma and its application to a pharmacokinetic study.

    Science.gov (United States)

    Chen, Jin Pei; Wang, Dian Lei; Yang, Li Li; Wang, Chen Yin; Wang, Shan Shan

    2014-12-01

    A highly sensitive and rapid ultra-high-performance liquid chromatography-tandem mass spectrometry method was developed and validated for the determination of gambogenic acid in dog plasma. Gambogic acid was used as an internal standard (IS). After a simple liquid-liquid extraction by ethyl acetate, the analyte and internal standard were separated on an Acquity BEH C18 (100 × 2.1 mm, 1.7 µm; Waters ) column at a flow rate of 0.2 mL/min, using 0.1% formic acid-methanol (10:90, v/v) as mobile phase. Electrospray ionization source was applied and operated in the positive ion mode. Multiple reaction monitoring mode with the transitions m/z 631.3 → 507.3 and m/z 629.1 → 573.2 was used to quantify gambogenic acid and the internal standard, respectively. The calibration curves were linear in the range of 5-1000 ng/mL, with a coefficient of determination (r) of 0.999 and good calculated accuracy and precision. The low limit of quantification was 5 ng/mL. The intra-and inter-day precisions (relative standard deviations) were dogs at a dose of 1 mg/kg. Copyright © 2014 John Wiley & Sons, Ltd.

  1. Simultaneous Quantitation of Free Amino Acids, Nucleosides and Nucleobases in Sipunculus nudus by Ultra-High Performance Liquid Chromatography with Triple Quadrupole Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Yahui Ge

    2016-03-01

    Full Text Available To evaluate the nutritional and functional value of Sipunculus nudus, a rapid, simple and sensitive analytical method was developed using ultra-high performance liquid chromatography coupled with a triple quadrupole mass detection in multiple-reaction monitoring mode for the simultaneous quantitative determination of 25 free amino acids and 16 nucleosides and nucleobases in S. nudus within 20 min, which was confirmed to be reproducible and accurate. The limits of detection (LODs and quantification (LOQs were between 0.003–0.229 μg/mL and 0.008–0.763 μg/mL for the 41 analytes, respectively. The established method was applied to analyze 19 batches of S. nudus samples from four habitats with two different processing methods. The results showed that S. nudus contained a variety of free amino acids, nucleosides and nucleobases in sufficient quantity and reasonable proportion. They also demonstrated that the contents of these compounds in different parts of S. nudus were significantly discriminating, which were in the order: (highest coelomic fluid > body wall > intestine (lowest. The method is simple and accurate, and could serve as a technical support for establishing quality control of S. nudus and other functional seafoods. Moreover, the research results also laid foundation for further exploitation and development of S. nudus.

  2. A simple and rapid ultra-high-performance liquid chromatography-tandem mass spectrometry method to determine plasma biotin in hemodialysis patients.

    Science.gov (United States)

    Yagi, Shigeaki; Nishizawa, Manabu; Ando, Itiro; Oguma, Shiro; Sato, Emiko; Imai, Yutaka; Fujiwara, Masako

    2016-08-01

    A simple, rapid, and selective method for determination of plasma biotin was developed using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). After single-step protein precipitation with methanol, biotin and stable isotope-labeled biotin as an internal standard (IS) were chromatographed on a pentafluorophenyl stationary-phase column (2.1 × 100 mm, 2.7 μm) under isocratic conditions using 10 mm ammonium formate-acetonitrile (93:7, v/v) at a flow rate of 0.6 mL/min. The total chromatographic runtime was 5 min for each injection. Detection was performed in a positive electrospray ionization mode by monitoring selected ion transitions at m/z 245.1/227.0 and 249.1/231.0 for biotin and the IS, respectively. The calibration curve was linear in the range of 0.05-2 ng/mL using 300 μL of plasma. The intra- and inter-day precisions were all biotin concentrations in hemodialysis patients. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  3. Determination of Fusarium toxins in functional vegetable milks applying salting-out-assisted liquid-liquid extraction combined with ultra-high-performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Hamed, Ahmed M; Arroyo-Manzanares, Natalia; García-Campaña, Ana M; Gámiz-Gracia, Laura

    2017-11-01

    Vegetable milks are considered as functional foods due to their physiological benefits. Although the consumption of these products has significantly increased, they have received little attention in legislation with regard to contaminants. However, they may contain mycotoxins resulting from the use of contaminated raw materials. In this work, ultra-high-performance liquid chromatography tandem mass spectrometry has been proposed for the determination of the most relevant Fusarium toxins (fumonisin B 1 and B 2 , HT-2 and T-2 toxins, zearalenone, deoxynivalenol and fusarenon-X) in different functional beverages based on cereals, legumes and seeds. Sample treatment consisted of a simple salting-out-assisted liquid-liquid extraction with no further clean-up. The method provided limits of quantification between 3.2 and 57.7 µg L -1 , recoveries above 80% and precision with RSD lower than 12%. The method was also applied for studying the occurrence of these mycotoxins in market samples of vegetable functional beverages and deoxynivalenol was found in three oat-based commercial drinks.

  4. Simultaneous determination of nitroimidazoles, benzimidazoles, and chloramphenicol components in bovine milk by ultra-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Wang, Yuanyuan; Li, Xiaowei; Zhang, Zhiwen; Ding, Shuangyang; Jiang, Haiyang; Li, Jiancheng; Shen, Jianzhong; Xia, Xi

    2016-02-01

    A sensitive, confirmatory ultra-high performance liquid chromatography-tandem mass spectrometric method was developed and validated to detect 23 veterinary drugs and metabolites (nitroimidazoles, benzimidazoles, and chloramphenicol components) in bovine milk. Compounds of interest were sequentially extracted from milk with acetonitrile and basified acetonitrile using sodium chloride to induce liquid-liquid partition. The extract was purified on a mixed mode solid-phase extraction cartridge. Using rapid polarity switching in electrospray ionization, a single injection was capable of detecting both positively and negatively charged analytes in a 9 min chromatography run time. Recoveries based on matrix-matched calibrations and isotope labeled internal standards for milk ranged from 51.7% to 101.8%. The detection limits and quantitation limits of the analytical method were found to be within the range of 2-20 ng/kg and 5-50 ng/kg, respectively. The recommended method is simple, specific, and reliable for the routine monitoring of nitroimidazoles, benzimidazoles, and chloramphenicol components in bovine milk samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

  5. Profiling and identification of (-)-epicatechin metabolites in rats using ultra-high performance liquid chromatography coupled with linear trap-Orbitrap mass spectrometer.

    Science.gov (United States)

    Shang, Zhanpeng; Wang, Fei; Dai, Shengyun; Lu, Jianqiu; Wu, Xiaodan; Zhang, Jiayu

    2017-08-01

    (-)-Epicatechin (EC), an optical antipode of (+)-catechin (C), possesses many potential significant health benefits. However, the in vivo metabolic pathway of EC has not been clarified yet. In this study, an efficient strategy based on ultra-high performance liquid chromatography coupled with a linear ion trap-Orbitrap mass spectrometer was developed to profile and characterize EC metabolites in rat urine, faeces, plasma, and various tissues. Meanwhile, post-acquisition data-mining methods including high-resolution extracted ion chromatogram (HREIC), multiple mass defect filters (MMDFs), and diagnostic product ions (DPIs) were utilized to screen and identify EC metabolites from HR-ESI-MS 1 to ESI-MS n stage. Finally, a total of 67 metabolites (including parent drug) were tentatively identified based on standard substances, chromatographic retention times, accurate mass measurement, and relevant drug biotransformation knowledge. The results demonstrated that EC underwent multiple in vivo metabolic reactions including methylation, dehydration, hydrogenation, glucosylation, sulfonation, glucuronidation, ring-cleavage, and their composite reactions. Among them, methylation, dehydration, glucosylation, and their composite reactions were observed only occurring on EC when compared with C. Meanwhile, the distribution of these detected metabolites in various tissues including heart, liver, spleen, lung, kidney, and brain were respectively studied. The results demonstrated that liver and kidney were the most important organs for EC and its metabolites elimination. In conclusion, the newly discovered EC metabolites significantly expanded the understanding on its pharmacological effects and built the foundation for further toxicity and safety studies. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  6. Wipe selection for the analysis of surface materials containing chemical warfare agent nitrogen mustard degradation products by ultra-high pressure liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Willison, Stuart A

    2012-12-28

    Degradation products arising from nitrogen mustard chemical warfare agent were deposited on common urban surfaces and determined via surface wiping, wipe extraction, and liquid chromatography–tandem mass spectrometry detection. Wipes investigated included cotton gauze, glass fiber filter, non-woven polyester fiber and filter paper, and surfaces included several porous (vinyl tile, painted drywall, wood) and mostly non-porous (laminate, galvanized steel, glass) surfaces. Wipe extracts were analyzed by ultra-high pressure liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) and compared with high performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) results. An evaluation of both techniques suggests UPLC–MS/MS provides a quick and sensitive analysis of targeted degradation products in addition to being nearly four times faster than a single HPLC run, allowing for greater throughput during a wide-spread release concerning large-scale contamination and subsequent remediation events. Based on the overall performance of all tested wipes, filter paper wipes were selected over other wipes because they did not contain interferences or native species (TEA and DEA) associated with the target analytes, resulting in high percent recoveries and low background levels during sample analysis. Other wipes, including cotton gauze, would require a pre-cleaning step due to the presence of large quantities of native species or interferences of the targeted analytes. Percent recoveries obtained from a laminate surface were 47–99% for all nitrogen mustard degradation products. The resulting detection limits achieved from wipes were 0.2 ng/cm(2) for triethanolamine (TEA), 0.03 ng/cm(2) for N-ethyldiethanolamine (EDEA), 0.1 ng/cm(2) for N-methyldiethanolamine (MDEA), and 0.1 ng/cm(2) for diethanolamine (DEA).

  7. Determination of oxycodone and its major metabolites noroxycodone and oxymorphone by ultra-high-performance liquid chromatography tandem mass spectrometry in plasma and urine: application to real cases.

    Science.gov (United States)

    Pantano, Flaminia; Brauneis, Stefano; Forneris, Alexandre; Pacifici, Roberta; Marinelli, Enrico; Kyriakou, Chrystalla; Pichini, Simona; Busardò, Francesco Paolo

    2017-08-28

    Oxycodone is a narcotic drug widely used to alleviate moderate and severe acute and chronic pain. Variability in analgesic efficacy could be explained by inter-subject variations in plasma concentrations of parent drug and its active metabolite, oxymorphone. To evaluate patient compliance and to set up therapeutic drug monitoring (TDM), an ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) assay was developed and validated for the parent drug and its major metabolites noroxycodone and oxymorphone. Extraction of analytes from plasma and urine samples was obtained by simple liquid-liquid extraction. The chromatographic separation was achieved with a reversed phase column using a linear gradient elution with two solvents: acetic acid 1% in water and methanol. The separated analytes were detected with a triple quadrupole mass spectrometer operated in multiple reaction monitoring (MRM) mode via positive electrospray ionization (ESI). Separation of analytes was obtained in less than 5 min. Linear calibration curves for all the analytes under investigation in urine and plasma samples showed determination coefficients (r2) equal or higher than 0.990. Mean absolute analytical recoveries were always above 86%. Intra- and inter-assay precision (measured as coefficient of variation, CV%) and accuracy (measured as % error) values were always better than 13%. Limit of detection at 0.06 and 0.15 ng/mL and limit of quantification at 0.2 and 0.5 ng/mL for plasma and urine samples, respectively, were adequate for the purpose of the present study. Rapid extraction, identification and quantification of oxycodone and its metabolites both in urine and plasma by UHPLC-MS/MS assay was tested for its feasibility in clinical samples and provided excellent results for rapid and effective drug testing in patients under oxycodone treatment.

  8. Analysis of Non-Volatile Chemical Constituents of Menthae Haplocalycis Herba by Ultra-High Performance Liquid Chromatography-High Resolution Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Lu-Lu Xu

    2017-10-01

    Full Text Available Menthae Haplocalycis herba, one kind of Chinese edible herbs, has been widely utilized for the clinical use in China for thousands of years. Over the last decades, studies on chemical constituents of Menthae Haplocalycis herba have been widely performed. However, less attention has been paid to non-volatile components which are also responsible for its medical efficacy than the volatile constituents. Therefore, a rapid and sensitive method was developed for the comprehensive identification of the non-volatile constituents in Menthae Haplocalycis herba using ultra-high performance liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometry (UHPLC-LTQ-Orbitrap. Separation was performed with Acquity UPLC® BEH C18 column (2.1 mm × 100 mm, 1.7 μm with 0.2% formic acid aqueous solution and acetonitrile as the mobile phase under gradient conditions. Based on the accurate mass measurement (<5 ppm, MS/MS fragmentation patterns and different chromatographic behaviors, a total of 64 compounds were unambiguously or tentatively characterized, including 30 flavonoids, 20 phenolic acids, 12 terpenoids and two phenylpropanoids. Finally, target isolation of three compounds named Acacetin, Rosmarinic acid and Clemastanin A (first isolated from Menthae Haplocalycis herba were performed based on the obtained results, which further confirmed the deduction of fragmentation patterns and identified the compounds profile in Menthae Haplocalycis herba. Our research firstly systematically elucidated the non-volatile components of Menthae Haplocalycis herba, which laid the foundation for further pharmacological and metabolic studies. Meanwhile, our established method was useful and efficient to screen and identify targeted constituents from traditional Chinese medicine extracts.

  9. Development of a new ultra-high performance liquid chromatography - tandem mass spectrometry method for determination of ambroxol hydrochloride in serum with pharmacokinetic application

    Directory of Open Access Journals (Sweden)

    Vujović Maja M.

    2016-01-01

    Full Text Available Ambroxol hydrochloride is an expectorant agent, successfully applied in mucolytic therapy for acute and chronic bronchopulmonary diseases. The drug regulates not only mucus secretion but also showed antioxidant, anti-inflammatory and local anesthetic properties. To supplement the pharmacokinetic and toxicological studies of ambroxol, a rapid ultra-high performance liquid chromatography-tandem mass spectrometry method for the quantitation of ambroxol in rabbit serum was developed. A validation of the method was performed as per the ICH guidelines for the validation of bioanalytical methods. The chromatographic separation was achieved in a submicron Kinetex RP - C18 - column (2.1 mm x 50 mm, 1.3μm using the no buffer mobile phase. The ESI mass spectrometry in the MRM mode was used with a typical transitions m/z 378.9→263.8 for ambroxol and m/z 455.2→165.0 for IS. Linearity was determined with an average coefficient of determination >0.999 over the dynamic range from 0.5 - 200 ng/mL with LOD and LOQ of 0.25 ng/mL and 0.5 ng/mL, respectively. The results of the intra- and inter-day precision and accuracy determined in different days were all found to be within the acceptable limits ±15%. The present method was successfully applied to pharmacokinetic study in the rabbits after a single oral dose administration. [Projekat Ministarstva nauke Republike Srbije, br. 175045

  10. Glycerolipid Profiling of Yellow Sarson Seeds Using Ultra High Performance Liquid Chromatography Coupled to Triple Time-of-Flight Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Shuning ZHENG

    2017-07-01

    Full Text Available Yellow sarson (Brassica rapa ssp. trillocularis is an important rapeseed-mustard species of Brassica rapa due to its high seed oil content. Glycerolipids and fatty acid composition affect seed germination and determine the quality of seed oil. To date, no information is available on the composition of individual glycerolipids in this species. Therefore, in this study the glycerolipid profiling of yellow sarson seeds was performed using ultra high performance liquid chromatography coupled to triple time-of-flight mass spectrometry (UPLC-Triple-TOF-MS. A fast and efficient chromatographic separation of glycerolipids was accomplished based on an UPLCTM BEH C8 column within 22 min. In ESI positive ion mode, TOF-MS scan-information dependent acquisition-product ion scan was carried out to acquire both high resolution MS and MS/MS information from one injection. According to MS/MS spectra, predominant fragmentation patterns of glycerolipids were elucidated in detail. Based on retention time, accurate mass, isotopic distribution, and fragmentation patterns, the composition of 144 glycerolipids and fatty acids were finally identified in yellow sarson seeds, including 77 triacylglycerols, 32 diacylglycerols, 18 sulfoquinovosyl-diacylglycerols, 5 monogalactosyl-diaclyglycerols, and 12 digalactosyl-diacylglycerols. Of them, the most abundant glycerolipids in yellow sarson seeds were triacylglycerols, the major storage form of seed oil in plants. In addition, diacylglycerols were found as a minor component of glycerolipids. The lowest amounts of glycerolipids detected in seeds were glycosyl-acylglycerols. The results revealed the composition and relative content of glycerolipids in yellow sarson seeds, which will provide a more comprehensive assessment of the quality of seed oil and also help to select functional cultivars with higher beneficial glycerolipids. This profiling method has the advantages of high throughput, high sensitivity and good accuracy

  11. Stable isotope dilution ultra-high performance liquid chromatography-tandem mass spectrometry quantitative profiling of tryptophan-related neuroactive substances in human serum and cerebrospinal fluid.

    Science.gov (United States)

    Hényková, Eva; Vránová, Hana Přikrylová; Amakorová, Petra; Pospíšil, Tomáš; Žukauskaitė, Asta; Vlčková, Magdaléna; Urbánek, Lubor; Novák, Ondřej; Mareš, Jan; Kaňovský, Petr; Strnad, Miroslav

    2016-03-11

    Many compounds related to L-tryptophan (L-TRP) have interesting biological or pharmacological activity, and their abnormal neurotransmission seems to be linked to a wide range of neurodegenerative and psychiatric diseases. A high-throughput method based on ultra-high performance liquid chromatography connected to electrospray tandem mass spectrometry (UHPLC-ESI-MS/MS) was developed for the quantitative analysis of L-TRP and 16 of its metabolites in human serum and cerebrospinal fluid (CSF), representing both major and minor routes of L-TRP catabolism. The combination of a fast LC gradient with selective tandem mass spectrometry enabled accurate analysis of almost 100 samples in 24h. The standard isotope dilution method was used for quantitative determination. The method's lower limits of quantification for serum and cerebrospinal fluid ranged from 0.05 to 15nmol/L and 0.3 to 45nmol/L, respectively. Analytical recoveries ranged from 10.4 to 218.1% for serum and 22.1 to 370.0% for CSF. The method's accuracy ranged from 82.4 to 128.5% for serum matrix and 90.7 to 127.7% for CSF matrix. All intra- and inter-day coefficients of variation were below 15%. These results demonstrate that the new method is capable of quantifying endogenous serum and CSF levels of a heterogeneous group of compounds spanning a wide range of concentrations. The method was used to determine the physiological levels of target analytes in serum and CSF samples from 18 individuals, demonstrating its reliability and potential usefulness in large-scale epidemiological studies. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Ultra-high-pressure liquid chromatography tandem mass spectrometry determination of antidepressant and anxiolytic drugs in neonatal meconium and maternal hair.

    Science.gov (United States)

    Pichini, Simona; Cortes, Laura; Marchei, Emilia; Solimini, Renata; Pacifici, Roberta; Gomez-Roig, Mª Dolores; García-Algar, Oscar

    2016-01-25

    A procedure based on ultra-high-pressure liquid chromatography tandem mass spectrometry has been developed for the determination of 22 antidepressant and anxiolytic drugs ad metabolites in the three consecutive maternal hair segments representing the pregnancy trimesters and paired neonatal meconium samples. After hair washing with methyl alcohol and diethyl ether and subsequent addition of internal standards, hair samples were treated with 500 μl VMA-T M3 reagent for 1h at 100 °C. After cooling, 100 μl M3 extract were diluted with 400 μl water and a volume of 10 μl was injected into chromatographic system. Meconium samples were firstly treated with 1 ml methyl alcohol and the organic layer back-extracted twice with 1.5 ml of a mixture of ethylacetate:hexane (80:20, v/v). Chromatographic separation was achieved at ambient temperature using a reverse-phase column and a linear gradient elution with two solvents: 0.3% formic acid in acetonitrile and 5mM ammonium formate pH 3. The mass spectrometer was operated in positive ion mode, using multiple reaction monitoring via positive electrospray ionization. The method was linear from the limit of quantification (0.05-1 ng/mg hair and 5-25 ng/g meconium depending on analyte under investigation;) to 10 ng/mg hair and 1000 ng/g meconium, with an intra- and inter-assay imprecision and inaccuracy always less than 20% and an analytical recovery between 66.6% and 95.3%, depending on the considered analyte and biological matrix. Using the validated method, 7 mothers were found positive to one or more hair segments and 5 meconium samples were found positive to one or more antidepressant and anxiolytic drugs, assessing prenatal exposure to these drugs following maternal consumption in one or more pregnancy trimesters. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Determination of caffeoylquinic acids in feed and related products by focused ultrasound solid-liquid extraction and ultra-high performance liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Tena, M T; Martínez-Moral, M P; Cardozo, P W

    2015-06-26

    A method to determine caffeoylquinic acids (CQAs) in three sources (herbal extract, feed additive and finished feed) using for the first time focused ultrasound solid-liquid extraction (FUSLE) followed by ultra-high performance liquid chromatography (UPLC) coupled to quadrupole-time of flight mass spectrometry is presented. Pressurized liquid extraction (PLE) was also tested as extraction technique but it was discarded because cynarin was not stable under temperature values used in PLE. The separation of the CQAs isomers was carried out in only seven minutes. FUSLE variables such as extraction solvent, power and time were optimized by a central composite design. Under optimal conditions, FUSLE extraction was performed with 8mL of an 83:17 methanol-water mixture for 30s at a power of 60%. Only two extraction steps were found necessary to recover analytes quantitatively. Sensitivity, linearity, accuracy and precision were established. Matrix effect was studied for each type of sample. It was not detected for mono-CQAs, whereas the cynarin signal was strongly decreased due to ionization suppression in presence of matrix components; so the quantification by standard addition was mandatory for the determination of di-caffeoylquinic acids. Finally, the method was applied to the analysis of herbal extracts, feed additives and finished feed. In all samples, chlorogenic acid was the predominant CQA, followed by criptochlorogenic acid, neochlorogenic acid and cynarin. The method allows an efficient determination of chlorogenic acid with good recovery rates. Therefore, it may be used for screening of raw material and for process and quality control in feed manufacture. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. A plasma metabonomic analysis on potential biomarker in pyrexia induced by three methods using ultra high performance liquid chromatography coupled with Fourier transform ion cyclotron resonance mass spectrometry.

    Science.gov (United States)

    Liu, Ting; Li, Songhe; Tian, Xiumin; Li, Zhaoqin; Cui, Yue; Han, Fei; Zhao, Yunli; Yu, Zhiguo

    2017-09-15

    Pyrexia usually is a systemic pathological process that can lead to metabolic disorders. Metabonomics as a powerful tool not only can reveal the pathological mechanisms, but also can give insight into the progression of pyrexia from another angle. Thus, an ultra high performance liquid chromatography combined with Fourier transform ion cyclotron resonance mass spectrometry (UHPLC-FT-ICR-MS) metabonomic approach was employed for the first time to investigate the plasma biochemical characteristics of pyrexia induced by three methods and to reveal subtle metabolic changes under the condition of pyrexia so as to explore its mechanism. The acquired metabolic data of the models were subjected to principal component analysis (PCA) for allowing the clear separation of the pyrexia rats from the control rats. Variable importance for project values (VIP) and Student's t-test were used to screen the significant metabolic changes caused by pyrexia. Fifty-two endogenous metabolites were identified and putatively identified as potential biomarkers primarily associated with phospholipid metabolism, sphingolipid metabolism, fatty acid oxidation metabolism, fatty acid amides metabolism and amino acid metabolism, and related to bile acid biosynthesis and glycerolipid catabolism. LysoPC (14:0), LysoPC (18:3), LysoPC (20:4), LysoPC (16:0), phytosphingosine, Cer (d18:0/12:0), N-[(4E,8E)-1,3-dihydroxyoctadeca-4,8-dien-2-yl]hexadecanamide, oleamide, fatty acid amide C22:1, tryptophan, acetylcarnitine, palmitoylcarnitine and stearoylcarnitine were considered as common potential biomarkers of pyrexia rats induced by three methods: Our results revealed that the UHPLC-FT-ICR-MS-based metabolomic method is helpful for finding new potential metabolic markers for pyrexia detection and offers a good perspective in pyrexia research. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Dried Blood Spots Combined With Ultra-High-Performance Liquid Chromatography-Mass Spectrometry for the Quantification of the Antipsychotics Risperidone, Aripiprazole, Pipamperone, and Their Major Metabolites.

    Science.gov (United States)

    Tron, Camille; Kloosterboer, Sanne M; van der Nagel, Bart C H; Wijma, Rixt A; Dierckx, Bram; Dieleman, Gwen C; van Gelder, Teun; Koch, Birgit C P

    2017-08-01

    Risperidone, aripiprazole, and pipamperone are antipsychotic drugs frequently prescribed for the treatment of comorbid behavioral problems in children with autism spectrum disorders. Therapeutic drug monitoring (TDM) could be useful to decrease side effects and to improve patient outcome. Dried blood spot (DBS) sample collection seems to be an attractive technique to develop TDM of these drugs in a pediatric population. The aim of this work was to develop and validate a DBS assay suitable for TDM and home sampling. Risperidone, 9-OH risperidone, aripiprazole, dehydroaripiprazole, and pipamperone were extracted from DBS and analyzed by ultra-high-performance liquid chromatography-tandem mass spectrometry using a C18 reversed-phase column with a mobile phase consisting of ammonium acetate/formic acid in water or methanol. The suitability of DBS for TDM was assessed by studying the influence of specific parameters: extraction solution, EDTA carryover, hematocrit, punching location, spot volume, and hemolysis. The assay was validated with respect to conventional guidelines for bioanalytical methods. The method was linear, specific without any critical matrix effect, and with a mean recovery around 90%. Accuracy and imprecision were within the acceptance criteria in samples with hematocrit values from 30% to 45%. EDTA or hemolysis did not skew the results, and no punching carryover was observed. No significant influence of the spot volume or the punch location was observed. The antipsychotics were all stable in DBS stored 10 days at room temperature and 1 month at 4 or -80°C. The method was successfully applied to quantify the 3 antipsychotics and their metabolites in patient samples. A UHPLC-MS/MS method has been successfully validated for the simultaneous quantification of risperidone, 9-OH risperidone, aripiprazole, dehydroaripiprazole, and pipamperone in DBS. The assay provided good analytical performances for TDM and clinical research applications.

  16. Determination of steroid hormones and their metabolite in several types of meat samples by ultra high performance liquid chromatography-Orbitrap high resolution mass spectrometry.

    Science.gov (United States)

    López-García, Marina; Romero-González, Roberto; Garrido Frenich, Antonia

    2018-03-09

    A new analytical method based on ultra-high performance liquid chromatography (UHPLC) coupled to Orbitrap high resolution mass spectrometry (Orbitrap-HRMS) has been developed for the determination of steroid hormones (hydrocortisone, cortisone, progesterone, prednisone, prednisolone, testosterone, melengesterol acetate, hydrocortisone-21-acetate, cortisone-21-acetate, testosterone propionate, 17α-methyltestosterone, 6α-methylprednisolone and medroxyprogesterone) and their metabolite (17α-hydroxyprogesterone) in three meat samples (chicken, pork and beef). Two different extraction approaches were tested (QuEChERS "quick, easy, cheap, effective, rugged and safe" and "dilute and shoot"), observing that the QuEChERS method provided the best results in terms of recovery. A clean-up step was applied comparing several sorbents, obtaining the best results when florisil and aluminum oxide were used. The optimized method was validated, obtaining suitable results for all validation parameters in the three meat matrices evaluated. Recovery values ranged from 70% to 103% (except for prednisone in beef samples), meanwhile repeatability and reproducibility were obtained at values lower than 18% and 21%, respectively. The limit of quantification (LOQ) was established for most of the compounds at 1.0 μg/kg, except for testosterone in chicken and hydrocortisone-21-acetate and cortisone-21-acetate in pork at 2.0 μg/kg. Decision limit (CCα) and detection capability (CCβ) values ranged from 1.0-2.7 μg/kg and 1.9-5.5 μg/kg, respectively, in the three matrices. Finally, thirty one meat samples were analyzed and two hormones, progesterone and hydrocortisone, were detected in a beef and pork sample at 1.7 and 2.8 μg/kg respectively. Copyright © 2018 Elsevier B.V. All rights reserved.

  17. Pre-column dilution large volume injection ultra-high performance liquid chromatography-tandem mass spectrometry for the analysis of multi-class pesticides in cabbages.

    Science.gov (United States)

    Zhong, Qisheng; Shen, Lingling; Liu, Jiaqi; Yu, Dianbao; Li, Siming; Yao, Jinting; Zhan, Song; Huang, Taohong; Hashi, Yuki; Kawano, Shin-ichi; Liu, Zhaofeng; Zhou, Ting

    2016-04-15

    Pre-column dilution large volume injection (PD-LVI), a novel sample injection technique for reverse phase ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), was developed in this study. The PD-LVI UHPLC-MS/MS system was designed by slightly modifying the commercial UHPLC-MS/MS equipment with a mixer chamber. During the procedure of PD-LVI, sample solution of 200μL was directly carried by the organic mobile phase to the mixer and diluted with the aqueous mobile phase. After the mixture was introduced to the UHPLC column in a mobile phase of acetonitrile-water (15/85, v/v), the target analytes were stacked on the head of the column until following separation. Using QuEChERS extraction, no additional steps such as solvent evaporation or residue redissolution were needed before injection. The features of PD-LVI UHPLC-MS/MS system were systematically investigated, including the injection volume, the mixer volume, the precondition time and the gradient elution. The efficiency of this approach was demonstrated by direct analysis of 24 pesticides in cabbages. Under the optimized conditions, low limits of detection (0.00074-0.8 ng/kg) were obtained. The recoveries were in the range of 63.3-109% with relative standard deviations less than 8.1%. Compared with common UHPLC-MS/MS technique, PD-LVI UHPLC-MS/MS showed significant advantages such as excellent sensitivity and reliability. The mechanism of PD-LVI was demonstrated to be based on the column-head stacking effect with pre-column dilution. Based on the results, PD-LVI as a simple and effective sample injection technique of reverse phase UHPLC-MS/MS for the analysis of trace analytes in complex samples showed a great promising prospect. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Ultra high performance liquid chromatography-tandem mass spectrometry vs. commercial immunoassay for determination of vancomycin plasma concentration in children. Possible implications for everyday clinical practice.

    Science.gov (United States)

    Barco, Sebastiano; Castagnola, Elio; Gennai, Iulian; Barbagallo, Laura; Loy, Anna; Tripodi, Gino; Cangemi, Giuliana

    2016-10-01

    Vancomycin therapeutic drug monitoring (TDM) is necessary for effective and safetherapy. The aim of the this paper was to develop a specific and robust ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for vancomycin quantification starting from low plasma volumes to be applied for the routine TDM in children. Samples from children receiving intravenous vancomycin were analysed using a TSQ Quantum Access MAX Triple Quadrupole system coupled with an Accela 1250 UHPLC system after a rapid protein precipitation. Gradient separation chromatography was carried out using a Hypersil GOLD aQ C18 column (50 × 2.1 mm, particle size 1.9 μm). Method performance was validated following international guidelines. UHPLC-MS/MS allowed a rapid and specific quantification of vancomycin over the range 0.1-128 μg/mL from 50 μL of plasma with high reproducibility and accuracy in the absence of matrix effect. The comparison with the commercial immunoassay performed on 138 samples demonstrated the presence of a proportional bias. The concentrations of vancomycin measured with immunoassay were found to be 4.5% (95% CI: 1.3-7.7) higher than those determined with UHPLC-MS/MS. Importantly, a clinical discordance was found in about 10% of samples analysed. This new UHPLC-MS/MS method is accurate and specific for the measurement of vancomycin starting from small (50 μL) plasma volumes. The use of UHPLC-MS/MS is recommended to prevent a misclassification of therapeutic or toxic vancomycin levels in paediatrics.

  19. The use of dried blood spots for quantification of 15 antipsychotics and 7 metabolites with ultra-high performance liquid chromatography - tandem mass spectrometry.

    Science.gov (United States)

    Patteet, Lisbeth; Maudens, Kristof E; Stove, Christophe P; Lambert, Willy E; Morrens, Manuel; Sabbe, Bernard; Neels, Hugo

    2015-06-01

    Therapeutic drug monitoring of antipsychotics is important in optimizing individual therapy. In psychiatric populations, classical venous blood sampling is experienced as frightening. Interest in alternative techniques, like dried blood spots (DBS), has consequently increased. A fast and easy to perform DBS method for quantification of 16 antipsychotics (amisulpride, aripiprazole, asenapine, bromperidol, clozapine, haloperidol, iloperidone, levosulpiride, lurasidone, olanzapine, paliperidone, pipamperone, quetiapine, risperidone, sertindole and zuclopenthixol) and 8 metabolites was developed. DBS were prepared using 25 μL of whole blood and extraction of complete spots was performed using methanol: methyl-t-butyl-ether (4:1). After evaporation, the extract was reconstituted in the mobile phase and 10 μL were injected on an ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Separation using a C18 column and gradient elution with a flow rate of 0.5 mL/min resulted in a 6-min run-time. Ionization was performed in positive mode and a dynamic MRM method was applied. Median recovery was 66.4 % (range 28.7-84.5%). Accuracy was within the acceptance criteria, except for pipamperone (LLOQ and low concentration) and lurasidone (low concentration). Imprecision was only aberrant for lurasidone at low and medium concentration. All compounds were stable during 1 month at room temperature, 4 °C and -18 °C. Lurasidone was unstable when the extract was stored for 12 h on the autosampler. Absolute matrix effects (ME) (median 66.1%) were compensated by the use of deuterated IS (median 98.8%). The DBS method was successfully applied on 25-μL capillary DBS from patients and proved to be a reliable alternative for quantification of all antipsychotics except for olanzapine and N-desmethylolanzapine. Copyright © 2014 John Wiley & Sons, Ltd.

  20. Strategy for Comprehensive Profiling and Identification of Acidic Glycosphingolipids Using Ultra-High-Performance Liquid Chromatography Coupled with Quadrupole Time-of-Flight Mass Spectrometry.

    Science.gov (United States)

    Hu, Ting; Jia, Zhixin; Zhang, Jin-Lan

    2017-07-18

    Acidic glycosphingolipids (AGSLs), which mainly consist of ganglioside and sulfatide moieties, are highly concentrated in the central nervous system. Comprehensive profiling of AGSLs has historically been challenging because of their high complexity and the lack of standards. In this study, a novel strategy was developed to comprehensively profile AGSLs using ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry. Ganglioside isomers with different glycan chains such as GD1a/GD1b were completely separated on a C18 column for the first time to our knowledge, facilitated by the addition of formic acid in the mobile phase. A mathematical model was established to predict the retention times (RTs) of all theoretically possible AGSLs on the basis of the good logarithmic relationship between the ceramide carbon numbers of the AGSLs in the reference material and their RTs. A data set was created of 571 theoretically possible AGSLs, including the ceramide carbon numbers, RTs, and high-resolution quasi-molecular ions. A novel fast identification strategy was established for global AGSL profiling by comparing the high-resolution quasi-molecular ions and RTs of the tested peaks to those in the data set of 571 AGSLs. Using this strategy, 199 AGSL candidates were identified in rat brain tissue. MS/MS fragments were further collected for these 199 candidates to confirm their identity as AGSLs. This novel strategy was employed to profile AGSLs in brain tissue samples from control rats and model rats with bilateral common carotid artery (2-VO) cerebral ischemia. Forty AGSLs were significantly different between the control and model groups, and these differences were further interpreted.

  1. Qualitative and quantitative analysis of an alkaloid fraction from Piper longum L. using ultra-high performance liquid chromatography-diode array detector-electrospray ionization mass spectrometry.

    Science.gov (United States)

    Li, Kuiyong; Fan, Yunpeng; Wang, Hui; Fu, Qing; Jin, Yu; Liang, Xinmiao

    2015-05-10

    In a previous research, an alkaloid fraction and 18 alkaloid compounds were prepared from Piper longum L. by series of purification process. In this paper, a qualitative and quantitative analysis method using ultra-high performance liquid chromatography-diode array detector-mass spectrometry (UHPLC-DAD-MS) was developed to evaluate the alkaloid fraction. Qualitative analysis of the alkaloid fraction was firstly completed by UHPLC-DAD method and 18 amide alkaloid compounds were identified. A further qualitative analysis of the alkaloid fraction was accomplished by UHPLC-MS/MS method. Another 25 amide alkaloids were identified according to their characteristic ions and neutral losses. At last, a quantitative method for the alkaloid fraction was established using four marker compounds including piperine, pipernonatine, guineensine and N-isobutyl-2E,4E-octadecadienamide. After the validation of this method, the contents of above four marker compounds in the alkaloid fraction were 57.5mg/g, 65.6mg/g, 17.7mg/g and 23.9mg/g, respectively. Moreover, the relative response factors of other three compounds to piperine were calculated. A comparative study between external standard quantification and relative response factor quantification proved no remarkable difference. UHPLC-DAD-MS method was demonstrated to be a powerful tool for the characterization of the alkaloid fraction from P. longum L. and the result proved that the quality of alkaloid fraction was efficiently improved after appropriate purification. Copyright © 2015. Published by Elsevier B.V.

  2. Determination of six microcystins and nodularin in surface and drinking waters by on-line solid phase extraction-ultra high pressure liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Beltrán, Eduardo; Ibáñez, María; Sancho, Juan Vicente; Hernández, Félix

    2012-11-30

    Microcystins and nodularin are cyclic peptides hepatotoxins produced by cyanobacterial genera (blue-green algae). Toxic cyanobacterial blooms are a worldwide problem, as reported in several countries, like China, Australia, or the United States. Therefore, it is necessary to develop sensitive and reliable analytical methodology to determine this type of toxins in water at parts per billion levels, or even lower. In this work, the potential of solid-phase extraction coupled on-line to ultra-high-pressure liquid chromatography/electrospray tandem mass spectrometry (SPE-UHPLC-MS/MS) has been investigated for the efficient quantification and confirmation of microcystins LR, RR, YR, LY, LW, LF and nodularin in surface and drinking water samples, at sub-ppb levels. The method developed involves the injection of only 1 mL of water sample into the on-line SPE-UHPLC-MS/MS system and allows the rapid determination of the compounds selected (8 min of chromatographic run), avoiding laborious sample treatment. The method was validated in surface and drinking water by means of recovery experiments at 0.25 and 1 μg L(-1). Average recoveries (n=5) ranged from 71 to 116%, with relative standard deviations (RSDs) lower than 15%. For microcystins LR, RR, YR and nodularin, a third level was also assayed (0.1 μg L(-1)) obtaining satisfactory data too. Limits of detection between 0.002 and 0.0405 μg L(-1) were estimated (0.0005 μg L(-1) for nodularin). The developed method was applied to the analysis of water samples collected in the province of Castellón (Spain). The acquisition of three MS/MS transitions for each compound allowed the unequivocal confirmation of positive samples, which was supported by the accomplishment of ion intensity ratios and retention time when compared with reference standards. Copyright © 2012 Elsevier B.V. All rights reserved.

  3. Development and validation of an ultra high performance liquid chromatography tandem mass spectrometry method for simultaneous determination of sulfonamides, quinolones and benzimidazoles in bovine milk.

    Science.gov (United States)

    Hou, Xiao-Lin; Chen, Guo; Zhu, Li; Yang, Ting; Zhao, Jian; Wang, Lei; Wu, Yin-Liang

    2014-07-01

    A simple, sensitive and reliable analytical method was developed for the simultaneous determination of 38 veterinary drugs (18 sulfonamides, 11 quinolones and 9 benzimidazoles) and 8 metabolites of benzimidazoles in bovine milk by ultra high performance liquid chromatography-positive electrospray ionization tandem mass spectrometry (UHPLC-ESI-MS/MS). Samples were extracted with acidified acetonitrile, cleaned up with Oasis(®) MCX cartridges, and analyzed by LC-MS/MS on an Acquity UPLC(®) BEH C18 column with gradient elution. The method allows such multi-analyte measurements within a 13min runtime while the specificity is ensured through the MRM acquisition mode. The method was validated according to the European Commission Decision 2002/657/EC determining specificity, decision limit (CCα), detection capability (CCβ), recovery, precision, linearity and stability. For compounds which have MRLs in bovine milk, the CCα values fall into a range from 11 to 115μg/kg, and the CCβ values fall within a range of 12-125μg/kg. For compounds which have not MRLs in bovine milk, the CCα values fall into a range from 0.01 to 0.08μg/kg, and the CCβ values fall within a range of 0.02-0.11μg/kg. The mean recoveries of the 46 analytes were between 87 and 119%. The calculated RSD values of repeatability and within-laboratory reproducibility experiments were below 11% and 15% for the 46 compounds, respectively. The method was demonstrated to be suitable for the simultaneous determination of sulfonamides, quinolones and benzimidazoles in bovine milk. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Decarboxylation Study of Acidic Cannabinoids: A Novel Approach Using Ultra-High-Performance Supercritical Fluid Chromatography/Photodiode Array-Mass Spectrometry

    Science.gov (United States)

    Wang, Mei; Wang, Yan-Hong; Avula, Bharathi; Radwan, Mohamed M.; Wanas, Amira S.; van Antwerp, John; Parcher, Jon F.; ElSohly, Mahmoud A.; Khan, Ikhlas A.

    2016-01-01

    Abstract Introduction: Decarboxylation is an important step for efficient production of the major active components in cannabis, for example, Δ9-tetrahydrocannabinol (Δ9-THC), cannabidiol (CBD), and cannabigerol (CBG). These cannabinoids do not occur in significant concentrations in cannabis but can be formed by decarboxylation of their corresponding acids, the predominant cannabinoids in the plant. Study of the kinetics of decarboxylation is of importance for phytocannabinoid isolation and dosage formulation for medical use. Efficient analytical methods are essential for simultaneous detection of both neutral and acidic cannabinoids. Methods: C. sativa extracts were used for the studies. Decarboxylation conditions were examined at 80°C, 95°C, 110°C, 130°C, and 145°C for different times up to 60 min in a vacuum oven. An ultra-high performance supercritical fluid chromatography/photodiode array-mass spectrometry (UHPSFC/PDA-MS) method was used for the analysis of acidic and neutral cannabinoids before and after decarboxylation. Results: Decarboxylation at different temperatures displayed an exponential relationship between concentration and time indicating a first-order or pseudo-first-order reaction. The rate constants for Δ9-tetrahydrocannabinolic acid-A (THCA-A) were twice those of the cannabidiolic acid (CBDA) and cannabigerolic acid (CBGA). Decarboxylation of THCA-A was forthright with no side reactions or by-products. Decarboxylation of CBDA and CBGA was not as straightforward due to the unexplained loss of reactants or products. Conclusion: The reported UHPSFC/PDA-MS method provided consistent and sensitive analysis of phytocannabinoids and their decarboxylation products and degradants. The rate of change of acidic cannabinoid concentrations over time allowed for determination of rate constants. Variations of rate constants with temperature yielded values for reaction energy. PMID:28861498

  5. Detection of anabolic and androgenic steroids and/or their esters in horse hair using ultra-high performance liquid chromatography-high resolution mass spectrometry.

    Science.gov (United States)

    Kwok, Karen Y; Choi, Timmy L S; Kwok, Wai Him; Wong, Jenny K Y; Wan, Terence S M

    2017-04-14

    Anabolic and androgenic steroids (AASs) are a class of prohibited substances banned in horseracing at all times. The common approach for controlling the misuse of AASs in equine sports is by detecting the presence of AASs and/or their metabolites in urine and blood samples using gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS). This approach, however, often falls short as the duration of effect for many AASs are longer than their detection time in both urine and blood. As a result, there is a high risk that such AASs could escape detection in their official race-day samples although they may have been used during the long period of training. Hair analysis, on the other hand, can afford significantly longer detection windows. In addition, the identification of synthetic ester derivatives of AASs in hair, particularly for the endogenous ones, can provide unequivocal proof of their exogenous origin. This paper describes the development of a sensitive method (at sub to low parts-per-billion or ppb levels) for detecting 48 AASs and/or their esters in horse hair using ultra-high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS). Decontaminated horse hair was pulverised and subjected to in-situ liquid-liquid extraction in a mixture of hexane - ethyl acetate (7:3, v/v) and phosphate buffer (0.1M, pH 9.5), followed by additional clean-up using mixed-mode solid-phase extraction. The final extract was analysed using UHPLC-HRMS in the positive electrospray ionisation (ESI) mode with both full scan and parallel reaction monitoring (PRM). This method was validated for qualitative identification purposes. Validation data, including method specificity, method sensitivity, extraction recovery, method precision and matrix effect are presented. Method applicability was demonstrated by the successful detection and confirmation of testosterone propionate in a referee hair sample. To our knowledge, this was

  6. Sensitive screening of abused drugs in dried blood samples using ultra-high-performance liquid chromatography-ion booster-quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Chepyala, Divyabharathi; Tsai, I-Lin; Liao, Hsiao-Wei; Chen, Guan-Yuan; Chao, Hsi-Chun; Kuo, Ching-Hua

    2017-03-31

    An increased rate of drug abuse is a major social problem worldwide. The dried blood spot (DBS) sampling technique offers many advantages over using urine or whole blood sampling techniques. This study developed a simple and efficient ultra-high-performance liquid chromatography-ion booster-quadrupole time-of-flight mass spectrometry (UHPLC-IB-QTOF-MS) method for the analysis of abused drugs and their metabolites using DBS. Fifty-seven compounds covering the most commonly abused drugs, including amphetamines, opioids, cocaine, benzodiazepines, barbiturates, and many other new and emerging abused drugs, were selected as the target analytes of this study. An 80% acetonitrile solvent with a 5-min extraction by Geno grinder was used for sample extraction. A Poroshell column was used to provide efficient separation, and under optimal conditions, the analytical times were 15 and 5min in positive and negative ionization modes, respectively. Ionization parameters of both electrospray ionization source and ion booster (IB) source containing an extra heated zone were optimized to achieve the best ionization efficiency of the investigated abused drugs. In spite of their structural diversity, most of the abused drugs showed an enhanced mass response with the high temperature ionization from an extra heated zone of IB source. Compared to electrospray ionization, the ion booster (IB) greatly improved the detection sensitivity for 86% of the analytes by 1.5-14-fold and allowed the developed method to detect trace amounts of compounds on the DBS cards. The validation results showed that the coefficients of variation of intra-day and inter-day precision in terms of the signal intensity were lower than 19.65%. The extraction recovery of all analytes was between 67.21 and 115.14%. The limits of detection of all analytes were between 0.2 and 35.7ngmL -1 . The stability study indicated that 7% of compounds showed poor stability (below 50%) on the DBS cards after 6 months of storage at

  7. Development and validation of an ultra-high performance liquid chromatography-tandem mass spectrometry method to measure creatinine in human urine.

    Science.gov (United States)

    Fraselle, S; De Cremer, K; Coucke, W; Glorieux, G; Vanmassenhove, J; Schepers, E; Neirynck, N; Van Overmeire, I; Van Loco, J; Van Biesen, W; Vanholder, R

    2015-04-15

    Despite decades of creatinine measurement in biological fluids using a large variety of analytical methods, an accurate determination of this compound remains challenging. Especially with the novel trend to assess biomarkers on large sample sets preserved in biobanks, a simple and fast method that could cope with both a high sample throughput and a low volume of sample is still of interest. In answer to these challenges, a fast and accurate ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed to measure creatinine in small volumes of human urine. In this method, urine samples are simply diluted with a basic mobile phase and injected directly under positive electrospray ionization (ESI) conditions, without further purification steps. The combination of an important diluting factor (10(4) times) due to the use of a very sensitive triple quadrupole mass spectrometer (XEVO TQ) and the addition of creatinine-d3 as internal standard completely eliminates matrix effects coming from the urine. The method was validated in-house in 2012 according to the EMA guideline on bioanalytical method validation using Certified Reference samples from the German External Quality Assessment Scheme (G-Equas) proficiency test. All obtained results for accuracy and recovery are within the authorized tolerance ranges defined by G-Equas. The method is linear between 0 and 5 g/L, with LOD and LOQ of 5 × 10(-3) g/L and 10(-2) g/L, respectively. The repeatability (CV(r) = 1.03-2.07%) and intra-laboratory reproducibility (CV(RW) = 1.97-2.40%) satisfy the EMA 2012 guideline. The validated method was firstly applied to perform the German G-Equas proficiency test rounds 51 and 53, in 2013 and 2014, respectively. The obtained results were again all within the accepted tolerance ranges and very close to the reference values defined by the organizers of the proficiency test scheme, demonstrating an excellent accuracy of the developed method. The

  8. Development of an isotope labeling ultra-high performance liquid chromatography mass spectrometric method for quantification of acylglycines in human urine

    Energy Technology Data Exchange (ETDEWEB)

    Stanislaus, Avalyn; Guo, Kevin [Department of Chemistry, University of Alberta, Edmonton, Alberta (Canada); Li Liang, E-mail: Liang.Li@ualberta.ca [Department of Chemistry, University of Alberta, Edmonton, Alberta (Canada)

    2012-10-31

    Graphical abstract: - Abstract: Acylglycines play a crucial regulatory and detoxification role in the accumulation of the corresponding acyl CoA esters and are an important class of metabolites in the diagnoses of inborn errors of metabolism. Sensitive quantification of a large number of acylglycines not only improves diagnosis but also enables the discovery of potential new biomarkers of diseases. We report an ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS) method for quantifying acylglycines in human urine with high sensitivity. This method is based on the use of a newly developed isotope labeling reagent, p-dimethylaminophenacyl (DmPA) bromide, to label acylglycines to improve detection sensitivity. Eighteen acylglycines, namely acetylglycine, propionylglycine, isobutyrylglycine, butyrylglycine, 4-hydroxyphenylacetylglycine, 2-furoylglycine, tiglylglycine, 2-methybutyrylglycine, 3-methylcrotonylglycine, isovalerylglycine, valerylglycine, hexanoylglycine, phenylacetylglycine, phenylpropionylglycine, glutarylglycine, heptanoylglycine, octanoylglycine and suberylglycine, were measured. This method uses calibration standards prepared in surrogate matrix (un-derivatized urine) and stable-isotope labeled analytes as the internal standards. The analysis was carried out in the positive ion detection mode using multiple reaction monitoring (MRM) survey scans. The calibration curves were validated over the range of 1.0-500 nM. The method achieved a lower limit of quantitation (LLOQ) of 1-5 nM for all analytes, as measured by the standard derivations associated with calibration curves and confirmed in surrogate matrix; the signal-to-noise ratio at LLOQ ranged from 12.50 to 156.70. Both accuracy (% RE or relative error) and precision (% CV) were <15%. Matrix effects were minimized using the surrogate matrix. All eighteen analytes were stable in urine for at least 5 h at room temperature, autosampler (4 Degree-Sign C) for 24 h, 7 weeks at -20

  9. Simultaneous Determination of Underivatized Vitamin B1 and B6 in Whole Blood by Reversed Phase Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry

    Science.gov (United States)

    Puts, Johan; de Groot, Monique; Haex, Martin; Jakobs, Bernadette

    2015-01-01

    Background Vitamin B1 (thiamine-diphosphate) and B6 (pyridoxal-5’phosphate) are micronutrients. Analysis of these micronutrients is important to diagnose potential deficiency which often occurs in elderly people due to malnutrition, in severe alcoholism and in gastrointestinal compromise due to bypass surgery or disease. Existing High Performance Liquid Chromatography (HPLC) based methods include the need for derivatization and long analysis time. We developed an Ultra High Performance Liquid Chromatography Tandem Mass spectrometry (UHPLC-MS/MS) assay with internal standards for simultaneous measurement of underivatized thiamine-diphosphate and pyridoxal-5’phosphate without use of ion pairing reagent. Methods Whole blood, deproteinized with perchloric acid, containing deuterium labelled internal standards thiamine-diphosphate(thiazole-methyl-D3) and pyridoxal-5’phosphate(methyl-D3), was analyzed by UHPLC-MS/MS. The method was validated for imprecision, linearity, recovery and limit of quantification. Alternate (quantitative) method comparisons of the new versus currently used routine HPLC methods were established with Deming regression. Results Thiamine-diphosphate and pyridoxal-5’phosphate were measured within 2.5 minutes instrumental run time. Limits of detection were 2.8 nmol/L and 7.8 nmol/L for thiamine-diphosphate and pyridoxal-5’phosphate respectively. Limit of quantification was 9.4 nmol/L for thiamine-diphosphate and 25.9 nmol/L for pyridoxal-5’phosphate. The total imprecision ranged from 3.5–7.7% for thiamine-diphosphate (44–157 nmol/L) and 6.0–10.4% for pyridoxal-5’phosphate (30–130 nmol/L). Extraction recoveries were 101–102% ± 2.5% (thiamine-diphosphate) and 98–100% ± 5% (pyridoxal-5’phosphate). Deming regression yielded slopes of 0.926 and 0.990 in patient samples (n = 282) and national proficiency testing samples (n = 12) respectively, intercepts of +3.5 and +3 for thiamine-diphosphate (n = 282 and n = 12) and slopes of

  10. Evaluation of cannabinoids concentration and stability in standardized preparations of cannabis tea and cannabis oil by ultra-high performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Pacifici, Roberta; Marchei, Emilia; Salvatore, Francesco; Guandalini, Luca; Busardò, Francesco Paolo; Pichini, Simona

    2017-08-28

    Cannabis has been used since ancient times to relieve neuropathic pain, to lower intraocular pressure, to increase appetite and finally to decrease nausea and vomiting. The combination of the psychoactive cannabis alkaloid Δ9-tetrahydrocannabinol (THC) with the non-psychotropic alkaloids cannabidiol (CBD) and cannabinol (CBN) demonstrated a higher activity than THC alone. The Italian National Institute of Health sought to establish conditions and indications on how to correctly use nationally produced cannabis to guarantee therapeutic continuity in individuals treated with medical cannabis. The evaluation of cannabinoids concentration and stability in standardized preparations of cannabis tea and cannabis oil was conducted using an easy and fast ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) assay. Extraction efficiency of oil was significantly higher than that of water with respect to the different cannabinoids. This was especially observed in the case of the pharmacologically active THC, CBD and their acidic precursors. Fifteen minutes boiling was sufficient to achieve the highest concentrations of cannabinoids in the cannabis tea solutions. At ambient temperature, a significant THC and CBD decrease to 50% or less of the initial concentration was observed over 3 and 7 days, respectively. When refrigerated at 4 °C, similar decreasing profiles were observed for the two compounds. The cannabinoids profile in cannabis oil obtained after pre-heating the flowering tops at 145 °C for 30 min in a static oven resulted in a complete decarboxylation of cannabinoid acids CBDA and THCA-A. Nevertheless, it was apparent that heat not only decarboxylated acidic compounds, but also significantly increased the final concentrations of cannabinoids in oil. The stability of cannabinoids in oil samples was higher than that in tea samples since the maximum decrease (72% of initial concentration) was observed in THC coming from unheated flowering

  11. Determination of fluorotelomer alcohols and their degradation products in biosolids-amended soils and plants using ultra-high performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Zhang, Hongna; Wen, Bei; Hu, Xiaoyu; Wu, Yali; Luo, Lei; Chen, Zien; Zhang, Shuzhen

    2015-07-24

    Degradation of fluorotelomer alcohols (FTOHs) was recognized as an additional source of perfluorocarboxylic acids (PFCAs). Quantification of FTOHs and their degradation products can help shed light on the sources and fates of PFCAs in the environment. In this study, an analytical method was developed for the determination of 6:2 and 8:2 FTOHs, and their degradation products of poly- and perfluorinated acids, including fluorotelomer saturated and unsaturated carboxylic acids (FTCAs and FTUCAs), secondary polyfluorinated alcohols and PFCAs in biosolids-amended soils and plants using ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The extract efficiencies of different methods including ethyl acetate and methanol (MeOH) for FTOHs and acetonitrile, MeOH, methyl tert-butyl ether (MTBE), NaOH-MeOH and NaOH-MTBE for poly- and perfluorinated acids were tested. The results showed that 6:2 and 8:2 FTOHs and their degradation products could be simultaneously and satisfactorily extracted by MeOH, cleaned up by Envi-Carb graphitized carbon and solid phase extraction, respectively, and determined by UPLC-MS/MS separately. NaOH in the extractant caused the conversion of 6:2 FTCA and 8:2 FTCA into the corresponding FTUCAs. The selected methods have matrix recoveries ranged from 52% to 102%, and detection limits of 0.01-0.46ng/g dry weight for FTOHs and their degradation products in soil and plant. The optimized method was applied successfully to quantify FTOHs and their degradation products in two biosolids-amended soils and plants. The total concentrations of FTOHs in the soils were 44.1±5.8 and 82.6±7.1ng/g, and in plants tissues 3.58±0.25 and 8.33±0.66ng/g. The total concentrations of poly- and perfluorinated acids in the soils were 168.0±13.2 and 349.6±11.2ng/g, and in plants tissues 78.0±6.4 and 75.5±5.3ng/g. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Ultra-high-performance liquid chromatography tandem mass spectrometry determination of GHB, GHB-glucuronide in plasma and cerebrospinal fluid of narcoleptic patients under sodium oxybate treatment.

    Science.gov (United States)

    Tittarelli, Roberta; Pichini, Simona; Pedersen, Daniel S; Pacifici, Roberta; Moresco, Monica; Pizza, Fabio; Busardò, Francesco Paolo; Plazzi, Giuseppe

    2017-05-01

    Sodium oxybate (Xyrem ® ), the sodium salt of γ- hydroxybutyric acid (GHB), is a first-line treatment of the symptoms induced by type 1 narcolepsy (NT1) and it is highly effective in improving sleep architecture, decreasing excessive daytime sleepiness and the frequency of cataplexy attacks. Using an ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) validated method, GHB was determined together with its glucuronide (GHB-gluc), in plasma and cerebrospinal fluid (CSF) samples of NT1 patients under sodium oxybate treatment. To characterize the plasma pharmacokinetics of GHB, three subjects with NT1 were administered at time 0 and 4h with 1.25, 1.5 and 3.55g Xyrem ® , respectively and had their blood samples collected at 7 time points throughout an 8-h session. CSF specimens, collected for orexin A measurement from the same three subjects 6h after their second administration, were also tested. The results obtained suggested that GHB plasma values increased disproportionally with the rising doses, (C max0-4 : 12.53, 32.95 and 69.62μg/mL; C max4-8 : 44.93, 75.03 and 111.93μg/mL for total Xyrem ® dose of 2.5, 3 and 7g respectively) indicating non-linear dose-response. GHB-Gluc was present only in traces in all plasma samples from treated patients, not changing with increasing Xyrem ® doses. GHB values of 5.62, 6.10 and 17.74μg/mL for 2, 3 and 7g Xyrem ® were found in CSF with a significant difference from control values. GHB-Gluc was found in negligible concentrations with no differences to those of control individuals. In conclusion this simple and fast UHPLC-MS/MS method proved useful for pharmacokinetic studies and therapeutic drug monitoring of GHB in narcoleptic patients treated with sodium oxybate. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Simultaneous Determination of Underivatized Vitamin B1 and B6 in Whole Blood by Reversed Phase Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry.

    Directory of Open Access Journals (Sweden)

    Johan Puts

    Full Text Available Vitamin B1 (thiamine-diphosphate and B6 (pyridoxal-5'phosphate are micronutrients. Analysis of these micronutrients is important to diagnose potential deficiency which often occurs in elderly people due to malnutrition, in severe alcoholism and in gastrointestinal compromise due to bypass surgery or disease. Existing High Performance Liquid Chromatography (HPLC based methods include the need for derivatization and long analysis time. We developed an Ultra High Performance Liquid Chromatography Tandem Mass spectrometry (UHPLC-MS/MS assay with internal standards for simultaneous measurement of underivatized thiamine-diphosphate and pyridoxal-5'phosphate without use of ion pairing reagent.Whole blood, deproteinized with perchloric acid, containing deuterium labelled internal standards thiamine-diphosphate(thiazole-methyl-D3 and pyridoxal-5'phosphate(methyl-D3, was analyzed by UHPLC-MS/MS. The method was validated for imprecision, linearity, recovery and limit of quantification. Alternate (quantitative method comparisons of the new versus currently used routine HPLC methods were established with Deming regression.Thiamine-diphosphate and pyridoxal-5'phosphate were measured within 2.5 minutes instrumental run time. Limits of detection were 2.8 nmol/L and 7.8 nmol/L for thiamine-diphosphate and pyridoxal-5'phosphate respectively. Limit of quantification was 9.4 nmol/L for thiamine-diphosphate and 25.9 nmol/L for pyridoxal-5'phosphate. The total imprecision ranged from 3.5-7.7% for thiamine-diphosphate (44-157 nmol/L and 6.0-10.4% for pyridoxal-5'phosphate (30-130 nmol/L. Extraction recoveries were 101-102% ± 2.5% (thiamine-diphosphate and 98-100% ± 5% (pyridoxal-5'phosphate. Deming regression yielded slopes of 0.926 and 0.990 in patient samples (n = 282 and national proficiency testing samples (n = 12 respectively, intercepts of +3.5 and +3 for thiamine-diphosphate (n = 282 and n = 12 and slopes of 1.04 and 0.84, intercepts of -2.9 and +20 for

  14. Rapid screening of anabolic steroids in horse urine with ultra-high-performance liquid chromatography/tandem mass spectrometry after chemical derivatisation.

    Science.gov (United States)

    Wong, Colton H F; Leung, David K K; Tang, Francis P W; Wong, Jenny K Y; Yu, Nola H; Wan, Terence S M

    2012-04-06

    Liquid chromatography/mass spectrometry (LC/MS) has been successfully applied to the detection of anabolic steroids in biological samples. However, the sensitive detection of saturated hydroxysteroids, such as androstanediols, by electrospray ionisation (ESI) is difficult because of their poor ability to ionise. In view of this, chemical derivatisation has been used to enhance the detection sensitivity of hydroxysteroids by LC/MS. This paper describes the development of a sensitive ultra-high-performance liquid chromatography/tandem mass spectrometry (UHPLC/MS/MS) method for the screening of anabolic steroids in horse urine by incorporating a chemical derivatisation step, using picolinic acid as the derivatisation reagent. The method involved solid-phase extraction (SPE) of both free and conjugated anabolic steroids in horse urine using a polymer-based SPE cartridge (Abs Elut Nexus). The conjugated steroids in the eluate were hydrolysed by methanolysis and the resulting extract was further cleaned up by liquid-liquid extraction. The resulting free steroids in the extract were derivatised with picolinic acid to form the corresponding picolinoyl esters and analysed by UHPLC/MS/MS in the positive ESI mode with selected-reaction-monitoring. Separation of the targeted steroids was performed on a C18 UHPLC column. The instrument turnaround time was 10.5 min inclusive of post-run equilibration. A total of thirty-three anabolic steroids (including 17β-estradiol, 5(10)-estrene-3β,17α-diol, 5α-estrane-3β,17α-diol, 17α-ethyl-5α-estran-3α,17β-diol, 17α-methyl-5α-androstan-3,17β-diols, androstanediols, nandrolone and testosterone) spiked in negative horse urine at the QC levels (ranging from 0.75 to 30 ng/mL) could be consistently detected. The intra-day and inter-day precisions (% RSD) for the peak area ratios were around 7-51% and around 1-72%, respectively. The intra-day and inter-day precisions (% RSD) for the relative retention times were both less than 1% for

  15. Theoretical resolving power of a radiofrequency mass spectrometer

    International Nuclear Information System (INIS)

    Coc, A.; Le Gac, R.; Saint Simon, M. de; Thibault, C.; Touchard, F.

    1988-01-01

    Radiofrequency mass spectrometers of L.G. Smith's type can reach a resolving power of 10 6 -10 7 and a precision of 10 -9 -10 -10 . The resolving power, shape of peaks and limitations are described. As an example, the spectrometer to be used in an experiment aimed at measuring the anti p/p mass ratio is considered. (orig.)

  16. Tissue-specific metabolite profiling of Cyperus rotundus L. rhizomes and (+)-nootkatone quantitation by laser microdissection, ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry, and gas chromatography-mass spectrometry techniques.

    Science.gov (United States)

    Jaiswal, Yogini; Liang, Zhitao; Guo, Ping; Ho, Hing-Man; Chen, Hubiao; Zhao, Zhongzhen

    2014-07-23

    Cyperus rotundus L. is a plant species commonly found in both India and China. The caused destruction of this plant is of critical concern for agricultural produce. Nevertheless, it can serve as a potential source of the commercially important sesquiterpenoid (+)-nootkatone. The present work describes comparative metabolite profiling and (+)-nootkatone content determination in rhizome samples collected from these two countries. Laser dissected tissues, namely, the cortex, hypodermal fiber bundles, endodermis, amphivasal vascular bundles, and whole rhizomes were analyzed by ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-QTOF MS). Gas chromatography-mass spectrometry (GC-MS) analysis was used for profiling of essential oil constituents and quantitation of (+)-nootkatone. The content of (+)-nootkatone was found to be higher in samples from India (30.47 μg/10 g) compared to samples from China (21.72 μg/10 g). The method was validated as per International Conference on Harmonisation (ICH) guidelines (Q2 R1). The results from this study can be applied for quality control and efficient utilization of this terpenoid-rich plant for several applications in food-based industries.

  17. Determination of type A trichothecenes in coix seed by magnetic solid-phase extraction based on magnetic multi-walled carbon nanotubes coupled with ultra-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Dong, Maofeng; Si, Wenshuai; Wang, Weimin; Bai, Bing; Nie, Dongxia; Song, Weiguo; Zhao, Zhihui; Guo, Yirong; Han, Zheng

    2016-09-01

    Magnetic solid-phase extraction (m-SPE) is a promising sample preparation approach due to its convenience, speed, and simplicity. For the first time, a rapid and reliable m-SPE approach using magnetic multi-walled carbon nanotubes (m-MWCNTs) as the adsorbent was proposed for purification of type A trichothecenes including T-2 toxins (T2), HT-2 toxins (HT-2), diacetoxyscirpenol (DAS), and neosolaniol (NEO) in coix seed. The m-MWCNTs were synthesized by assembling the magnetic nanoparticles (Fe3O4) with MWCNTs by sonication through an aggregation wrap mechanism, and characterized by transmission electron microscope. Several key parameters affecting the performance of the procedure were extensively investigated including extraction solutions, desorption solvents, and m-MWCNT amounts. Under the optimal sample preparation conditions followed by analysis with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), high sensitivity (limit of quantification in the range of 0.3-1.5 μg kg(-1)), good linearity (R (2) > 0.99), satisfactory recovery (73.6-90.6 %), and acceptable precision (≤2.5 %) were obtained. The analytical performance of the developed method has also been successfully evaluated in real coix seed samples. Graphical Abstract Flow chart of determination of type A trichothecenes in coix seed by magnetic solid-phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry.

  18. Determination and fingerprint analysis of steroidal saponins in roots of Liriope muscari (Decne.) L. H. Bailey by ultra high performance liquid chromatography coupled with ion trap time-of-flight mass spectrometry.

    Science.gov (United States)

    Li, Yong-Wei; Qi, Jin; Wen-Zhang; Zhou, Shui-Ping; Yan-Wu; Yu, Bo-Yang

    2014-07-01

    Liriope muscari (Decne.) L. H. Bailey is a well-known traditional Chinese medicine used for treating cough and insomnia. There are few reports on the quality evaluation of this herb partly because the major steroid saponins are not readily identified by UV detectors and are not easily isolated due to the existence of many similar isomers. In this study, a qualitative and quantitative method was developed to analyze the major components in L. muscari (Decne.) L. H. Bailey roots. Sixteen components were deduced and identified primarily by the information obtained from ultra high performance liquid chromatography with ion-trap time-of-flight mass spectrometry. The method demonstrated the desired specificity, linearity, stability, precision, and accuracy for simultaneous determination of 15 constituents (13 steroidal glycosides, 25(R)-ruscogenin, and pentylbenzoate) in 26 samples from different origins. The fingerprint was established, and the evaluation was achieved using similarity analysis and principal component analysis of 15 fingerprint peaks from 26 samples by ultra high performance liquid chromatography. The results from similarity analysis were consistent with those of principal component analysis. All results suggest that the established method could be applied effectively to the determination of multi-ingredients and fingerprint analysis of steroid saponins for quality assessment and control of L. muscari (Decne.) L. H. Bailey. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Hardon cross sections at ultra high energies

    International Nuclear Information System (INIS)

    Yodh, G.B.

    1987-01-01

    A review of results on total hadronic cross sections at ultra high energies obtained from a study of longitudinal development of cosmic ray air showers is given. The experimental observations show that proton-air inelastic cross section increases from 275 mb to over 500 mb as the collision energy in the center of mass increases from 20 GeV to 20 TeV. The proton-air inelastic cross section, obtained from cosmic ray data at √s = 30 TeV, is compared with calculations using various different models for the energy variation of the parameters of the elementary proton-proton interaction. Three conclusions are derived

  20. Fe- and Cu-complex formation with artificial ligands investigated by ultra-high resolution Fourier-transform ion cyclotron resonance mass spectrometry (FT-ICR-MS: Implications for natural metal-organic complex studies

    Directory of Open Access Journals (Sweden)

    Hannelore Waska

    2016-07-01

    Full Text Available In recent years, electrospray-ionization mass spectrometry (ESI-MS has been increasingly used to complement the bulk determination of metal-ligand equilibria, for example via competitive ligand exchange-adsorptive cathodic stripping voltammetry (CLE-ACSV. However, ESI-MS speciation analyses may be impacted by instrumental artefacts such as reduction reactions, fragmentation, and adduct formation at the ESI source, changes in the ionization efficiencies of the detected species in relation to sample matrix, and peak overlaps in response to increasing sample complexity. In our study, equilibria of the known artificial ligands citrate, ethylenediaminetetraacetic acid (EDTA, 1-nitroso-2-naphthol (NN, and salicylaldoxime (SA with iron (Fe and copper (Cu were investigated by ultra-high resolution ESI-MS, Fourier-transform ion cyclotron resonance mass spectrometry (FT-ICR-MS, under a variety of sample matrix and ionization settings. The acquired mass spectra were compared with metal-ligand equilibrium data from the literature as well as an adapted speciation model. Overall, the mass spectra produced representative species mentioned in previous reports and predicted by the speciation calculations, such as Fe(Cit, Cu(Cit2, Fe(EDTA, Cu(EDTA, Fe(NN3, and Cu(SA2. The analyses furthermore revealed new species which had been hypothesized but not measured directly using other methods, for example ternary complexes of citrate with Fe and Cu, Cu(SA monomers, and the dimer Fe(SA2. Finally, parallel measurements of a Cu+SA calibration series and a Cu+SA+EDTA competition series indicated that FT-ICR-MS can produce linear responses and low detection limits analogous to those of ACSV. We propose that ultra-high resolution FT-ICR-MS can be used as a representative tool to study interactions of trace metals with artificial as well as natural, unknown ligands at the molecular level.

  1. Ultra-high-performance liquid chromatography/tandem high-resolution mass spectrometry analysis of sixteen red beverages containing carminic acid: identification of degradation products by using principal component analysis/discriminant analysis.

    Science.gov (United States)

    Gosetti, Fabio; Chiuminatto, Ugo; Mazzucco, Eleonora; Mastroianni, Rita; Marengo, Emilio

    2015-01-15

    The study investigates the sunlight photodegradation process of carminic acid, a natural red colourant used in beverages. For this purpose, both carminic acid aqueous standard solutions and sixteen different commercial beverages, ten containing carminic acid and six containing E120 dye, were subjected to photoirradiation. The results show different patterns of degradation, not only between the standard solutions and the beverages, but also from beverage to beverage. Due to the different beverage recipes, unpredictable reactions take place between the dye and the other ingredients. To identify the dye degradation products in a very complex scenario, a methodology was used, based on the combined use of principal component analysis with discriminant analysis and ultra-high-performance liquid chromatography coupled with tandem high resolution mass spectrometry. The methodology is unaffected by beverage composition and allows the degradation products of carminic acid dye to be identified for each beverage. Copyright © 2014 Elsevier Ltd. All rights reserved.

  2. Development of filter element from nanocomposites of ultra high molar mass polyethylene having silver nanoparticles; Desenvolvimento de elemento filtrante a partir de nanocompositos de polietileno de ultra-alta massa molar contendo nanoparticulas de prata

    Energy Technology Data Exchange (ETDEWEB)

    Bizzo, Maurizio A.; Wang, S. Hui, E-mail: mbizzo@usp.br [Universidade de Sao Paulo (USP), Sao Paulo, SP (Brazil). Escola Politecnica de Engenharia Metalurgica e de Materiais

    2015-07-01

    The production of polymer based filter elements for water is widespread in the market but has an undesirable characteristic, they are not always efficient and capable of retaining or eliminating microorganisms. This paper proposes the production of filters with biocidal activity, comprised by nanocomposites of ultra-high molar mass polyethylene (UHMMPE) containing silver nanoparticles. The polymer is responsible for the uniform porous structure of the filter element and the Ag nanoparticles for its biocidal action. The filter elements were produced from two kinds of UHMMPE particles with different particle size distributions, one in the range of 150 to 200μm and the other of 300 to 400μm. Samples were collected from the obtained filter elements and characterized by X-ray diffractometry, scanning electron microscopy and microanalysis. The results indicated the formation of nanocomposite containing silver nanoparticles. (author)

  3. Characterization of phenolic and other polar compounds in peel and flesh of pink guava (Psidium guajava L. cv. 'Criolla') by ultra-high performance liquid chromatography with diode array and mass spectrometric detection.

    Science.gov (United States)

    Rojas-Garbanzo, Carolina; Zimmermann, Benno F; Schulze-Kaysers, Nadine; Schieber, Andreas

    2017-10-01

    Pink guava (Psidium guajava L.) is a highly consumed fruit in tropical countries. Despite of interesting research on health effects of this fruit, investigations into the profile of secondary plant metabolites are scarce. In this study, the phenolic compounds in the peel and flesh of pink guava were characterized by ultra-high performance liquid chromatography with diode array and mass spectrometric detection. Sixty phenolic compounds were characterized by MS 2 and classified as ellagitannins, flavones, flavonols, flavanols, proanthocyanidins, dihydrochalcones, and anthocyanidins, and non-flavonoids such as phenolic acid derivatives, stilbenes, acetophenones, and benzophenones. Forty-two polyphenols are reported for the first time in both peel and flesh, and twenty-four compounds were detected for the first time in P. guajava, e.g., phlorizin, nothofagin, astringin, chrysin-C-glucoside, valoneic acid bilactone, cinnamoyl-glucoside, and two dimethoxycinnamoyl-hexosides. Copyright © 2016 Elsevier Ltd. All rights reserved.

  4. Analysis of the Constituents in “Zhu She Yong Xue Shuan Tong” by Ultra High Performance Liquid Chromatography with Quadrupole Time-of-Flight Mass Spectrometry Combined with Preparative High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Lin-Lin Wang

    2015-11-01

    Full Text Available “Zhu She Yong Xue Shuan Tong” lyophilized powder (ZSYXST, consists of a series of saponins extracted from Panax notoginseng, which has been widely used in China for the treatment of strokes. In this study, an ultra-high performance liquid chromatography with quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF/MS combined with preparative high performance liquid chromatography (PHPLC method was developed to rapidly identify both major and minor saponins in ZSYXST. Some high content components were removed through PHPLC in order to increase the sensitivity of the trace saponins. Then, specific characteristic fragment ions in both positive and negative mode were utilized to determine the types of aglycone, saccharide, as well as the saccharide chain linkages. As a result, 94 saponins, including 20 pairs of isomers and ten new compounds, which could represent higher than 98% components in ZSYXST, were identified or tentatively identified in commercial ZSYXST samples.

  5. Determination of bovine lactoferrin in dairy products by ultra-high performance liquid chromatography–tandem mass spectrometry based on tryptic signature peptides employing an isotope-labeled winged peptide as internal standard

    International Nuclear Information System (INIS)

    Zhang, Jingshun; Lai, Shiyun; Cai, Zengxuan; Chen, Qi; Huang, Baifen; Ren, Yiping

    2014-01-01

    Highlights: • A UHPLC–MS/MS method for quantification of bovine lactoferrin was developed. • Tryptic fragment LRPVAAEIYGTK was chosen as signature peptide of bovine lactoferrin. • A winged peptide containing isotopically-labeled signature peptide was designed as internal standard. • The method for determining lactoferrin does not discriminate between the different forms of lactoferrin. • Meet the growing demand to quantify bovine lactoferrin in different dairy products. - Abstract: A new and sensitive determination method was developed for bovine lactoferrin in dairy products including infant formulas based on the signature peptide by ultra high-performance liquid chromatography and triple-quadrupole tandem mass spectrometry under the multiple reaction monitoring mode. The simple pretreatment procedures included the addition of a winged peptide containing the isotope-labeled signature peptide as internal standard, followed by an enzymatic digestion with trypsin. The signature peptide was chosen and identified from the tryptic hydrolyzates of bovine lactoferrin by ultra high-performance liquid chromatography and quadrupole-time-of-flight tandem mass spectrometry based on sequence database search. Analytes were separated on an ACQUITY UPLC BEH 300 C18 column and monitored by MS/MS in seven minutes. Quantitative result bias due to matrix effect and tryptic efficiency was corrected through the use of synthetic isotope-labeled standards. The limit of detection and limit of quantification were 0.3 mg/100 g and 1.0 mg/100 g, respectively. Bovine lactoferrin within the concentration range of 10–1000 nmol L −1 showed a strong linear relationship with a linear correlation coefficient (r) of >0.998. The intra- and inter-day precision of the method were RSD < 6.5% and RSD < 7.1%, respectively. Excellent repeatability (RSD < 6.4%) substantially supported the application of this method for the determination of bovine lactoferrin in dairy samples. The present

  6. Determination of bovine lactoferrin in dairy products by ultra-high performance liquid chromatography–tandem mass spectrometry based on tryptic signature peptides employing an isotope-labeled winged peptide as internal standard

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Jingshun [Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051 (China); Lai, Shiyun [Beingmate Research Institute, Beingmate Baby and Child Food Co., Ltd., Hangzhou 310007 (China); Cai, Zengxuan [Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051 (China); Chen, Qi [Beingmate Research Institute, Beingmate Baby and Child Food Co., Ltd., Hangzhou 310007 (China); Huang, Baifen [Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051 (China); Ren, Yiping, E-mail: renyiping@263.net [Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051 (China)

    2014-06-01

    Highlights: • A UHPLC–MS/MS method for quantification of bovine lactoferrin was developed. • Tryptic fragment LRPVAAEIYGTK was chosen as signature peptide of bovine lactoferrin. • A winged peptide containing isotopically-labeled signature peptide was designed as internal standard. • The method for determining lactoferrin does not discriminate between the different forms of lactoferrin. • Meet the growing demand to quantify bovine lactoferrin in different dairy products. Abstract: A new and sensitive determination method was developed for bovine lactoferrin in dairy products including infant formulas based on the signature peptide by ultra high-performance liquid chromatography and triple-quadrupole tandem mass spectrometry under the multiple reaction monitoring mode. The simple pretreatment procedures included the addition of a winged peptide containing the isotope-labeled signature peptide as internal standard, followed by an enzymatic digestion with trypsin. The signature peptide was chosen and identified from the tryptic hydrolyzates of bovine lactoferrin by ultra high-performance liquid chromatography and quadrupole-time-of-flight tandem mass spectrometry based on sequence database search. Analytes were separated on an ACQUITY UPLC BEH 300 C18 column and monitored by MS/MS in seven minutes. Quantitative result bias due to matrix effect and tryptic efficiency was corrected through the use of synthetic isotope-labeled standards. The limit of detection and limit of quantification were 0.3 mg/100 g and 1.0 mg/100 g, respectively. Bovine lactoferrin within the concentration range of 10–1000 nmol L⁻¹ showed a strong linear relationship with a linear correlation coefficient (r) of >0.998. The intra- and inter-day precision of the method were RSD < 6.5% and RSD < 7.1%, respectively. Excellent repeatability (RSD < 6.4%) substantially supported the application of this method for the determination of bovine lactoferrin in dairy samples. The present method

  7. Ultra high energy cosmic rays

    International Nuclear Information System (INIS)

    Watson, A.A.

    1986-01-01

    Cosmic radiation was discovered 70 years ago but its origin remains an open question. The background to this problem is outlined and attempts to discover the origin of the most energetic and rarest group above 10 15 eV are described. Measurements of the energy spectrum and arrival direction pattern of the very highest energy particles, mean energy about 6 x 10 19 eV, are used to argue that these particles originate outside our galaxy. Recent evidence from the new field of ultra high energy γ-ray astronomy are discussed in the context of a galactic origin hypothesis for lower energy cosmic rays. (author)

  8. A strategy for fast screening and identification of sulfur derivatives in medicinal Pueraria species based on the fine isotopic pattern filtering method using ultra-high-resolution mass spectrometry

    International Nuclear Information System (INIS)

    Yang, Min; Zhou, Zhe; Guo, De-an

    2015-01-01

    Sulfurous compounds are commonly present in plants, fungi, and animals. Most of them were reported to possess various bioactivities. Isotopic pattern filter (IPF) is a powerful tool for screening compounds with distinct isotope pattern. Over the past decades, the IPF was used mainly to study Cl- and Br-containing compounds. To our knowledge, the algorithm was scarcely used to screen S-containing compounds, especially when combined with chromatography analyses, because the "3"4S isotopic ion is drastically affected by "1"3C_2 and "1"8O. Thus, we present a new method for a fine isotopic pattern filter (FIPF) based on the separated M + 2 ions ("1"2C_x"1H_y"1"6O_z"3"2S"1"3C_2"1"8O, "1"2C_x_+_2"1H_y"1"6O_z_+_1"3"4S, tentatively named M + 2OC and M + 2S) with an ultra-high-resolution mass (100,000 FWHM @ 400 m/z) to screen sulfur derivatives in traditional Chinese medicines (TCM).This finer algorithm operates through convenient filters, including an accurate mass shift of M + 2OC and M + 2S from M and their relative intensity compared to M. The method was validated at various mass resolutions, mass accuracies, and screening thresholds of flexible elemental compositions. Using the established FIPF method, twelve S-derivatives were found in the popular medicinal used Pueraria species, and 9 of them were tentatively identified by high-resolution multiple stage mass spectrometry (HRMS"n). The compounds were used to evaluate the sulfurous compounds' situation in commercially purchased Pueraria products. The strategy presented here provides a promising application of the IPF method in a new field. - Highlights: • We provide a new strategy for specifically screening of sulfurous compounds. • The fine isotopic pattern filter (FIPF) bases on separation of "1"3C_2+"1"8O and "3"4S. • Ultra high resolution mass (100,000 FWHM @ 400 m/z) is essential for FIPF. • IPF is applied to study the unique components of TCM for the first time. • New sulfurous components

  9. A strategy for fast screening and identification of sulfur derivatives in medicinal Pueraria species based on the fine isotopic pattern filtering method using ultra-high-resolution mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Min [National Engineering Laboratory for TCM Standardization Technology, Shanghai Institute of Materia Medica, Chinese Academy of Sciences, 501 Haike Road, Shanghai 201203 (China); Zhou, Zhe [ThermoFisher Scientific China Co., Ltd, No 6 Building, 27 Xinjinqiao Road, Shanghai 201206 (China); Guo, De-an, E-mail: daguo@simm.ac.cn [National Engineering Laboratory for TCM Standardization Technology, Shanghai Institute of Materia Medica, Chinese Academy of Sciences, 501 Haike Road, Shanghai 201203 (China)

    2015-09-24

    Sulfurous compounds are commonly present in plants, fungi, and animals. Most of them were reported to possess various bioactivities. Isotopic pattern filter (IPF) is a powerful tool for screening compounds with distinct isotope pattern. Over the past decades, the IPF was used mainly to study Cl- and Br-containing compounds. To our knowledge, the algorithm was scarcely used to screen S-containing compounds, especially when combined with chromatography analyses, because the {sup 34}S isotopic ion is drastically affected by {sup 13}C{sub 2} and {sup 18}O. Thus, we present a new method for a fine isotopic pattern filter (FIPF) based on the separated M + 2 ions ({sup 12}C{sub x}{sup 1}H{sub y}{sup 16}O{sub z}{sup 32}S{sup 13}C{sub 2}{sup 18}O, {sup 12}C{sub x+2}{sup 1}H{sub y}{sup 16}O{sub z+1}{sup 34}S, tentatively named M + 2OC and M + 2S) with an ultra-high-resolution mass (100,000 FWHM @ 400 m/z) to screen sulfur derivatives in traditional Chinese medicines (TCM).This finer algorithm operates through convenient filters, including an accurate mass shift of M + 2OC and M + 2S from M and their relative intensity compared to M. The method was validated at various mass resolutions, mass accuracies, and screening thresholds of flexible elemental compositions. Using the established FIPF method, twelve S-derivatives were found in the popular medicinal used Pueraria species, and 9 of them were tentatively identified by high-resolution multiple stage mass spectrometry (HRMS{sup n}). The compounds were used to evaluate the sulfurous compounds' situation in commercially purchased Pueraria products. The strategy presented here provides a promising application of the IPF method in a new field. - Highlights: • We provide a new strategy for specifically screening of sulfurous compounds. • The fine isotopic pattern filter (FIPF) bases on separation of {sup 13}C{sub 2}+{sup 18}O and {sup 34}S. • Ultra high resolution mass (100,000 FWHM @ 400 m/z) is essential

  10. Ultra high performance liquid chromatography coupled with electrospray ionization/quadrupole time-of-flight mass spectrometry for the rapid analysis of constituents in the traditional Chinese medicine formula Wu Ji Bai Feng Pill.

    Science.gov (United States)

    Duan, Shengnan; Qi, Wen; Zhang, Siwen; Huang, Kunkun; Yuan, Dan

    2017-10-01

    An ultra high performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight mass spectrometry method in both positive and negative ion modes was established in order to comprehensively investigate the major constituents in Wu Ji Bai Feng Pill. Briefly, a Waters ACQUITY UPLC HSS C 18 column was used to separate the aqueous extract of Wu Ji Bai Feng Pill. A total of 0.1% formic acid in acetonitrile and 0.1% aqueous formic acid v/v were used as the mobile phase. All analytes were determined using quadrupole time-of-flight mass spectrometry with electrospray ionization source in positive and negative ion modes. At length, a total of 173 components including flavones and their glycosides, monoterpene glycosides, triterpene saponins, phenethylalchohol glycosides, iridoid glycosides, phthalides, tanshinones, phenolic acids, sesquiterpenoids and cyclopeptides were identified or tentatively characterized in Wu Ji Bai Feng Pill in an analysis of 16.0 min based on the accurate mass and tandem mass spectrometry behaviors. The developed method is rapid and highly sensitive to characterize the chemical constituents of Wu Ji Bai Feng Pill, which could not only be used for chemical standardization and quality control of Wu Ji Bai Feng Pill, but also be helpful for further study in vivo metabolism of Wu Ji Bai Feng Pill. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Characterization of phenolic amides from cortex lycii by ultra high-performance liquid chromatography coupled with LTQ-Orbitrap mass spectrometry

    Science.gov (United States)

    High performance liquid chromatography (UPLC) and flow injection electrospray ionization with ion trap mass spectrometry (FIMS) fingerprints combined with the principal component analysis (PCA) were examined for their potential in differentiating commercial organic and conventional sage samples. The...

  12. 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.

  13. Dispersive solid phase extraction combined with ion-pair ultra high-performance liquid chromatography tandem mass spectrometry for quantification of nucleotides in Lactococcus lactis

    DEFF Research Database (Denmark)

    Magdenoska, Olivera; Martinussen, Jan; Thykær, Jette

    2013-01-01

    solid phase extraction with charcoal and subsequent analysis with ion-pair liquid chromatography coupled with electrospray ionization tandem mass spectrometry was established for quantification of intracellular pools of the 28 most important nucleotides. The method can handle extracts where cells leak...

  14. Ultra-high performance supercritical fluid chromatography hyphenated to atmospheric pressure chemical ionization high resolution mass spectrometry for the characterization of fast pyrolysis bio-oils.

    Science.gov (United States)

    Crepier, Julien; Le Masle, Agnès; Charon, Nadège; Albrieux, Florian; Duchene, Pascal; Heinisch, Sabine

    2018-06-01

    Extensive characterization of complex mixtures requires the combination of powerful analytical techniques. A Supercritical Fluid Chromatography (SFC) method was previously developed, for the specific case of fast pyrolysis bio oils, as an alternative to gas chromatography (GC and GC × GC) or liquid chromatography (LC and LC × LC), both separation methods being generally used prior to mass spectrometry (MS) for the characterization of such complex matrices. In this study we investigated the potential of SFC hyphenated to high resolution mass spectrometry (SFC-HRMS) for this characterization using Negative ion Atmospheric Pressure Chemical ionization ((-)APCI) for the ionization source. The interface between SFC and (-)APCI/HRMS was optimized from a mix of model compounds with the objective of maximizing the signal to noise ratio. The main studied parameters included both make-up flow-rate and make-up composition. A methodology for the treatment of APCI/HRMS data is proposed. This latter allowed for the identification of molecular formulae. Both SFC-APCI/HRMS method and data processing method were applied to a mixture of 36 model compounds, first analyzed alone and then spiked in a bio-oil. In both cases, 19 compounds could be detected. Among them 9 could be detected in a fast pyrolysis bio-oil by targeted analysis. The whole procedure was applied to the characterization of a bio-oil using helpful representations such as mass-plots, van Krevelen diagrams and heteroatom class distributions. Finally the results were compared with those obtained with a Fourier Transform ion-cyclotron resonance mass spectrometer (FT-ICR/MS). Copyright © 2018 Elsevier B.V. All rights reserved.

  15. Use of ultra-high pressure liquid chromatography coupled to high resolution mass spectrometry for fast screening in high throughput doping control.

    Science.gov (United States)

    Musenga, Alessandro; Cowan, David A

    2013-05-03

    We describe a sensitive, comprehensive and fast screening method based on liquid chromatography-high resolution mass spectrometry for the detection of a large number of analytes in sports samples. UHPLC coupled to high resolution mass spectrometry with polarity switching capability is applied for the rapid screening of a large number of analytes in human urine samples. Full scan data are acquired alternating both positive and negative ionisation. Collision-induced dissociation with positive ionisation is also performed to produce fragment ions to improve selectivity for some analytes. Data are reviewed as extracted ion chromatograms based on narrow mass/charge windows (±5ppm). A simple sample preparation method was developed, using direct enzymatic hydrolysis of glucuronide conjugates, followed by solid phase extraction with mixed mode ion-exchange cartridges. Within a 10min run time (including re-equilibration) the method presented allows for the analysis of a large number of analytes from most of the classes in the World Anti-Doping Agency (WADA) Prohibited List, including anabolic agents, β2-agonists, hormone antagonists and modulators, diuretics, stimulants, narcotics, glucocorticoids and β-blockers, and does so while meeting the WADA sensitivity requirements. The high throughput of the method and the fast sample pre-treatment reduces analysis cost and increases productivity. The method presented has been used for the analysis of over 5000 samples in about one month and proved to be reliable. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Identification of metabolites in human and rat urine after oral administration of Xiao-Qing-Long-Tang granule using ultra high performance liquid chromatography combined with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Zhou, Lei; Zhang, Qiang; Qi, Wen; Yan, Shuai; Qu, Jialin; Makino, Toshiaki; Yuan, Dan

    2017-09-01

    Xiao-Qing-Long-Tang is a traditional Chinese formula used for the treatment of cold syndrome, bronchitis, and nasal allergies for thousands of years. However, the in vivo integrated metabolism of its multiple components and the active chemical constituents of Xiao-Qing-Long-Tang remain unknown. In this study, a method using ultra high performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry was established for the detection and identification of the metabolites in human and rat urine after oral administration of Xiao-Qing-Long-Tang. A total of 19 compounds were detected or tentatively identified in human urine samples, including eight prototypes and 11 metabolites. Also, a total of 50 compounds were detected or tentatively identified in rat urine samples, including 15 prototypes and 35 metabolites detected with either a highly sensitive extracted ion chromatogram method or the MS E determination using Mass Fragment software. Our results indicated that phase Ⅱ reactions (e.g. glucuronidation and sulfation) were the main metabolic pathways of flavones, while phase I reactions (e.g. demethylation and hydroxylation) were the major metabolic reaction for alkaloids, lignans, and ginger essential oil. This investigation provided important structural information on the metabolism of Xiao-Qing-Long-Tang and provided evidence to obtain a more comprehensive metabolic profile. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. A rapid method for simultaneous determination of 52 marker compounds in Xiao-Qing-Long-Tang by ultra high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Zhou, Lei; Qi, Wen; Xu, Cong; Makino, Toshiaki; Yuan, Dan

    2014-11-01

    Xiao-Qing-Long-Tang (XQLT) is a classical Chinese medicine formula. It is generally used for the treatment of common cold, bronchial asthma, and allergic rhinitis in Asia. In this study, a multicomponent quantification fingerprinting approach based on ultra high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry has been developed for the analysis of compounds in XQLT in 14.5 min. A total of 52 compounds were identified by co-chromatography of sample extract with authentic standards and comparing the retention time, UV spectra, molecular ions and characteristic fragment ions with those of authentic standards, or tentatively identified by MS(E) determination along with Mass Fragment software. Moreover, the method was validated for the simultaneous quantification of 16 components in XQLT commercial products. The method is practical for comprehensive standardization of XQLT and holistic comparison of its commercial products from different manufacturers. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. 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).

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

    Science.gov (United States)

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

    2016-03-11

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

  20. Identification and analysis of chemical constituents and rat serum metabolites in Suan-Zao-Ren granule using ultra high performance liquid chromatography quadrupole time-of-flight mass spectrometry combined with multiple data processing approaches.

    Science.gov (United States)

    Du, Yiyang; He, Bosai; Li, Qing; He, Jiao; Wang, Di; Bi, Kaishun

    2017-07-01

    Suan-Zao-Ren granule is widely used to treat insomnia in China. However, because of the complexity and diversity of the chemical compositions in traditional Chinese medicine formula, the comprehensive analysis of constituents in vitro and in vivo is rather difficult. In our study, an ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry and the PeakView® software, which uses multiple data processing approaches including product ion filter, neutral loss filter, and mass defect filter, method was developed to characterize the ingredients and rat serum metabolites in Suan-Zao-Ren granule. A total of 101 constituents were detected in vitro. Under the same analysis conditions, 68 constituents were characterized in rat serum, including 35 prototype components and 33 metabolites. The metabolic pathways of main components were also illustrated. Among them, the metabolic pathways of timosaponin AI were firstly revealed. The bioactive compounds mainly underwent the phase I metabolic pathways including hydroxylation, oxidation, hydrolysis, and phase II metabolic pathways including sulfate conjugation, glucuronide conjugation, cysteine conjugation, acetycysteine conjugation, and glutathione conjugation. In conclusion, our results showed that this analysis approach was extremely useful for the in-depth pharmacological research of Suan-Zao-Ren granule and provided a chemical basis for its rational. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Hyphenation of ultra high performance supercritical fluid chromatography with atmospheric pressure chemical ionisation high resolution mass spectrometry: Part 1. Study of the coupling parameters for the analysis of natural non-polar compounds.

    Science.gov (United States)

    Duval, Johanna; Colas, Cyril; Pecher, Virginie; Poujol, Marion; Tranchant, Jean-François; Lesellier, Eric

    2017-08-04

    An analytical method based on Ultra-High-Performance Supercritical Fluid Chromatography (UHPSFC) coupled with Atmospheric Pressure Chemical Ionization - High-resolution mass spectrometry (APCI-Q-TOF-HRMS) was developed for compounds screening from oily samples. The hyphenation was made using a commercial UHPLC device coupled to a CO 2 pump in order to perform the chromatographic analysis. An adaptation of the injection system for compressible fluids was accomplished for this coupling: this modification of the injection sequence was achieved to prevent unusual variations of the injected volume related to the use of a compressible fluid. UHPSFC-HRMS hyphenation was optimized to enhance the response of the varied compounds from a seed extract (anthraquinones, free fatty acids, diacylglycerols, hydroxylated triacylglycerols and triacylglycerols). No split was used prior to the APCI ionization source, allowing introducing all the compounds in the spectrometer, ensuring a better sensitivity for minor compounds. The effects of a mechanical make-up (T-piece) added before this ionization source was discussed in terms of standard deviation of response, response intensity and fragmentation percentage. The location of the T-piece with regards to the backpressure regulator (BPR), the flow rate and the nature of the make-up solvent were studied. Results show that the effects of the studied parameters depend on the nature of the compounds, whereas the make-up addition favours the robustness of the mass response (quantitative aspect). Copyright © 2017 Elsevier B.V. All rights reserved.

  2. A simultaneous screening and quantitative method for the multiresidue analysis of pesticides in spices using ultra-high performance liquid chromatography-high resolution (Orbitrap) mass spectrometry.

    Science.gov (United States)

    Goon, Arnab; Khan, Zareen; Oulkar, Dasharath; Shinde, Raviraj; Gaikwad, Suresh; Banerjee, Kaushik

    2018-01-12

    A novel screening and quantitation method is reported for non-target multiresidue analysis of pesticides using ultra-HPLC-quadrupole-Orbitrap mass spectrometry in spice matrices, including black pepper, cardamom, chili, coriander, cumin, and turmeric. The method involved sequential full-scan (resolution = 70,000), and variable data independent acquisition (vDIA) with nine consecutive fragmentation events (resolution = 17,500). Samples were extracted by the QuEChERS method. The introduction of an SPE-based clean-up step through hydrophilic-lipophilic-balance (HLB) cartridges proved advantageous in minimizing the false negatives. For coriander, cumin, chili, and cardamom, the screening detection limit was largely at 2 ng/g, while it was 5 ng/g for black pepper, and turmeric. When the method was quantitatively validated for 199 pesticides, the limit of quantification (LOQ) was mostly at 10 ng/g (excluding black pepper, and turmeric with LOQ = 20 ng/g) with recoveries within 70-120%, and precision-RSDs <20%. Furthermore, the method allowed the identification of suspected non-target analytes through retrospective search of the accurate mass of the compound-specific precursor and product ions. Compared to LC-MS/MS, the quantitative performance of this Orbitrap-MS method had agreements in residue values between 78-100%. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Determination of selected endogenous anabolic androgenic steroids and ratios in urine by ultra high performance liquid chromatography tandem mass spectrometry and isotope pattern deconvolution.

    Science.gov (United States)

    Pitarch-Motellón, J; Sancho, J V; Ibáñez, M; Pozo, O; Roig-Navarro, A F

    2017-09-15

    An isotope dilution mass spectrometry (IDMS) method for the determination of selected endogenous anabolic androgenic steroids (EAAS) in urine by UHPLC-MS/MS has been developed using the isotope pattern deconvolution (IPD) mathematical tool. The method has been successfully validated for testosterone, epitestosterone, androsterone and etiocholanolone, employing their respective deuterated analogs using two certified reference materials (CRM). Accuracy was evaluated as recovery of the certified values and ranged from 75% to 108%. Precision was assessed in intraday (n=5) and interday (n=4) experiments, with RSDs below 5% and 10% respectively. The method was also found suitable for real urine samples, with limits of detection (LOD) and quantification (LOQ) below the normal urinary levels. The developed method meets the requirements established by the World Anti-Doping Agency for the selected steroids for Athlete Biological Passport (ABP) measurements, except in the case of androsterone, which is currently under study. Copyright © 2017. Published by Elsevier B.V.

  4. Multi-constituent determination and fingerprint analysis of Scutellaria indica L. using ultra high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Liang, Xianrui; Zhao, Cui; Su, Weike

    2015-11-01

    An ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry method integrating multi-constituent determination and fingerprint analysis has been established for quality assessment and control of Scutellaria indica L. The optimized method possesses the advantages of speediness, efficiency, and allows multi-constituents determination and fingerprint analysis in one chromatographic run within 11 min. 36 compounds were detected, and 23 of them were unequivocally identified or tentatively assigned. The established fingerprint method was applied to the analysis of ten S. indica samples from different geographic locations. The quality assessment was achieved by using principal component analysis. The proposed method is useful and reliable for the characterization of multi-constituents in a complex chemical system and the overall quality assessment of S. indica. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Particle spectra and mass composition in the ultra-high energy region in the framework of the Galactic origin of cosmic rays

    Directory of Open Access Journals (Sweden)

    Lagutin A.A.

    2017-01-01

    Full Text Available The possibility for a self-consistent description of all the basic features of the observed cosmic ray spectra and primary composition variations in the energy range of 1015 ÷ 1020 eV within the Galactic origin scenario is examined. We assume the existence of Galactic sources that accelerate particles up to ∼ 3 · 1018Z eV and take into account a highly inhomogeneous (fractal-like distribution of matter and magnetic fields in the Galaxy that leads to extremely large free paths of particles (“Lévy flights”, along with an overwhelming contribution to the cosmic ray fluxes observed above ∼1018 eV from particles reaching the Solar System without scattering. Our scenario was refined on the basis of recent experimental results on primary mass composition. Model predictions, which could be verified with the improved high-precision measurements in the nearest future are discussed.

  6. Reversed-phase ultra-high-performance liquid chromatography coupled to electrospray ionization-quadrupole-time-of-flight mass spectrometry as a powerful tool for metabolic profiling of vegetables: Lactuca sativa as an example of its application.

    Science.gov (United States)

    Abu-Reidah, I M; Contreras, M M; Arráez-Román, D; Segura-Carretero, A; Fernández-Gutiérrez, A

    2013-10-25

    Lettuce (Lactuca sativa), a leafy vegetal widely consumed worldwide, fresh cut or minimally processed, constitutes a major dietary source of natural antioxidants and bioactive compounds. In this study, reversed-phase ultra-high-performance liquid chromatography (RP-UHPLC) coupled to electrospray ionization-quadrupole-time-of-flight mass spectrometry (ESI-QTOF-MS) was applied for the comprehensive profiling of polar and semi-polar metabolites from three lettuce cultivars (baby, romaine, and iceberg). The UHPLC systems allowed the use of a small-particle-size C18 column (1.8 μm), with very fine resolution for the separation of up to seven isomers, and the QTOF mass analyzer enabled sensitive detection with high mass resolution and accuracy in full scan. Thus, a total of 171 compounds were tentatively identified by matching their accurate mass signals and suggested molecular formula with those previously reported in family Asteraceae. Afterwards, their structures were also corroborated by the MS/MS data provided by the QTOF analyzer. Well-known amino acids, organic acids, sesquiterpene lactones, phenolic acids and flavonoids were characterized, e.g. lactucin, lactucopicrin, caftaric acid, chlorogenic acid, caffeoylmalic acid, chicoric acid, isochlorogenic acid A, luteolin, and quercetin glycosides. For this plant species, this is the first available report of several isomeric forms of the latter polyphenols and other types of components such as nucleosides, peptides, and tryptophan-derived alkaloids. Remarkably, 10 novel structures formed by the conjugation of known amino acids and sesquiterpene lactones were also proposed. Thus, the methodology applied is a useful option to develop an exhaustive metabolic profiling of plants that helps to explain their potential biological activities and folk uses. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. Ultra-high energy cosmic rays and prompt TeV gamma rays from ...

    Indian Academy of Sciences (India)

    physics pp. 789-792. Ultra-high energy cosmic rays and prompt. TeV gamma rays from gamma ray bursts ... The origin of the observed ultra-high energy cosmic ray (UHECR) events with ... are proton and electron rest mass, respectively.

  8. Screening of HIV-1 Protease Using a Combination of an Ultra-High-Throughput Fluorescent-Based Assay and RapidFire Mass Spectrometry.

    Science.gov (United States)

    Meng, Juncai; Lai, Ming-Tain; Munshi, Vandna; Grobler, Jay; McCauley, John; Zuck, Paul; Johnson, Eric N; Uebele, Victor N; Hermes, Jeffrey D; Adam, Gregory C

    2015-06-01

    HIV-1 protease (PR) represents one of the primary targets for developing antiviral agents for the treatment of HIV-infected patients. To identify novel PR inhibitors, a label-free, high-throughput mass spectrometry (HTMS) assay was developed using the RapidFire platform and applied as an orthogonal assay to confirm hits identified in a fluorescence resonance energy transfer (FRET)-based primary screen of > 1 million compounds. For substrate selection, a panel of peptide substrates derived from natural processing sites for PR was evaluated on the RapidFire platform. As a result, KVSLNFPIL, a new substrate measured to have a ~ 20- and 60-fold improvement in k cat/K m over the frequently used sequences SQNYPIVQ and SQNYPIV, respectively, was identified for the HTMS screen. About 17% of hits from the FRET-based primary screen were confirmed in the HTMS confirmatory assay including all 304 known PR inhibitors in the set, demonstrating that the HTMS assay is effective at triaging false-positives while capturing true hits. Hence, with a sampling rate of ~7 s per well, the RapidFire HTMS assay enables the high-throughput evaluation of peptide substrates and functions as an efficient tool for hits triage in the discovery of novel PR inhibitors. © 2015 Society for Laboratory Automation and Screening.

  9. Quantification and characterization of alkaloids from roots of Rauwolfia serpentina using ultra-high performance liquid chromatography-photo diode array-mass spectrometry.

    Science.gov (United States)

    Sagi, Satyanarayanaraju; Avula, Bharathi; Wang, Yan-Hong; Khan, Ikhlas A

    2016-01-01

    A new UHPLC-UV method has been developed for the simultaneous analysis of seven alkaloids [ajmaline (1), yohimbine (2), corynanthine (3), ajmalicine (4), serpentine (5), serpentinine (6), and reserpine (7)] from the root samples of Rauwolfia serpentina (L.) Benth. ex Kurz. The chromatographic separation was achieved using a reversed phase C18 column with a mobile phase of water and acetonitrile, both containing 0.05% formic acid. The seven compounds were completely separated within 8 min at a flow rate of 0.2 mL/min with a 2-μL injection volume. The method is validated for linearity, accuracy, repeatability, limits of detection (LOD), and limits of quantification (LOQ). Seven plant samples and 21 dietary supplements claiming to contain Rauwolfia roots were analyzed and content of total alkaloids (1-7) varied, namely, 1.57-12.1 mg/g dry plant material and 0.0-4.5 mg/day, respectively. The results indicated that commercial products are of variable quality. The developed analytical method is simple, economic, fast, and suitable for quality control analysis of Rauwolfia samples and commercial products. The UHPLC-QToF-mass spectrometry with electrospray ionization (ESI) interface method is described for the confirmation and characterization of alkaloids from plant samples. This method involved the detection of [M + H](+) or M(+) ions in the positive mode.

  10. Quantification of Lansoprazole in Oral Suspension by Ultra-High-Performance Liquid Chromatography Hybrid Ion-Trap Time-of-Flight Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Stacy D. Brown

    2011-01-01

    Full Text Available An LC-MS/MS method was developed and validated to be used as a stability indicating assay for the study of a 3 mg/mL lansoprazole oral suspension. The method utilizes a UPLC (ultra-performance liquid chromatography column and unique mass spectrometric detection (ion-trap time-of-flight (IT-TOF to achieve a sensitive (LOD 2 ng/mL, accurate, and reproducible quantification of lansoprazole. This method reports an intraday and interday coefficient of variation of 2.98 ± 2.17% (n=5 for each concentration for each day and 3.07 ± 0.89% (n=20 for each concentration, respectively. Calibration curves (5–25 μg/mL were found to be linear with an R2 value ranging from 0.9972 to 0.9991 on 4 different days. Accuracy of the assay, expressed as % error, ranged from 0.30 to 5.22%. This method is useful for monitoring the stability of lansoprazole in oral suspension.

  11. Metabolic profiles of neratinib in rat by using ultra-high-performance liquid chromatography coupled with diode array detector and Q-Exactive Orbitrap tandem mass spectrometry.

    Science.gov (United States)

    Liu, Wen; Li, Sha; Wu, Yangke; Yan, Xiao; Zhu, Y-M; Huang, J-H; Chen, Zhuo

    2018-05-03

    Neratinib is a tyrosine kinase inhibitor that has been approved by the US Food and Drug Administration for the treatment of breast cancer. However, its metabolism remains unknown. This study was carried out to investigate the in vitro and in vivo metabolism of neratinib using an UHPLC-DAD-Q Exactive Orbitrap-MS instrument with dd-MS 2 on-line data acquisition mode. The post-acquisition data was processed using MetWorks software. Under the current conditions, a total of 12 metabolites were detected and structurally identified based on their accurate masses, fragment ions and chromatographic retention times. Among these metabolites, M3, M10 and M12 were unambiguously identified using chemically synthesized reference standards. M6 and M7 (GSH conjugates) were the major metabolites. The metabolic pathways of neratinib were proposed accordingly. Our findings suggested that neratinib was mainly metabolized via O-dealkylation (M3), oxygenation (M8), N-demethylation (M10), N-oxygenation (M12), GSH conjugation (M1, M2, M4, M5, M6 and M7) and N-acetylcysteine conjugation (M9 and M11). The α,β-unsaturated ketone was the major metabolic site and GSH conjugation was the predominant metabolic pathway. In conclusion, this study provided valuable metabolic data and would benefit the assessment of the contributions to the overall activity or toxicity from the key metabolites. Copyright © 2018 John Wiley & Sons, Ltd.

  12. Ultra High Power and Efficiency Space Traveling-Wave Tube Amplifier Power Combiner with Reduced Size and Mass for NASA Missions

    Science.gov (United States)

    Simons, Rainee N.; Wintucky, Edwin G.; Wilson, Jeffrey D.; Force, Dale A.

    2009-01-01

    In the 2008 International Microwave Symposium (IMS) Digest version of our paper, recent advances in high power and efficiency space traveling-wave tube amplifiers (TWTAs) for NASA s space-to-Earth communications are presented. The RF power and efficiency of a new K-Band amplifier are 40 W and 50 percent and that of a new Ka-Band amplifier are 200 W and 60 percent. An important figure-of-merit, which is defined as the ratio of the RF power output to the mass (W/kg) of a TWT, has improved by a factor of ten over the previous generation Ka-Band devices. In this extended paper, a high power, high efficiency Ka-band combiner for multiple TWTs, based on a novel hybrid magic-T waveguide circuit design, is presented. The measured combiner efficiency is as high as 90 percent. In addition, at the design frequency of 32.05 GHz, error-free uncoded BPSK/QPSK data transmission at 8 megabits per second (Mbps), which is typical for deep space communications is demonstrated. Furthermore, QPSK data transmission at 622 Mbps is demonstrated with a low bit error rate of 2.4x10(exp -8), which exceeds the deep space state-of-the-art data rate transmission capability by more than two orders of magnitude. A potential application of the TWT combiner is in deep space communication systems for planetary exploration requiring transmitter power on the order of a kilowatt or higher.

  13. Validation of an ultra-high-performance liquid chromatography-tandem mass spectrometry method to quantify illicit drug and pharmaceutical residues in wastewater using accuracy profile approach.

    Science.gov (United States)

    Hubert, Cécile; Roosen, Martin; Levi, Yves; Karolak, Sara

    2017-06-02

    The analysis of biomarkers in wastewater has become a common approach to assess community behavior. This method is an interesting way to estimate illicit drug consumption in a given population: by using a back calculation method, it is therefore possible to quantify the amount of a specific drug used in a community and to assess the consumption variation at different times and locations. Such a method needs reliable analytical data since the determination of a concentration in the ngL -1 range in a complex matrix is difficult and not easily reproducible. The best analytical method is liquid chromatography - mass spectrometry coupling after solid-phase extraction or on-line pre-concentration. Quality criteria are not specially defined for this kind of determination. In this context, it was decided to develop an UHPLC-MS/MS method to analyze 10 illicit drugs and pharmaceuticals in wastewater treatment plant influent or effluent using a pre-concentration on-line system. A validation process was then carried out using the accuracy profile concept as an innovative tool to estimate the probability of getting prospective results within specified acceptance limits. Influent and effluent samples were spiked with known amounts of the 10 compounds and analyzed three times a day for three days in order to estimate intra-day and inter-day variations. The matrix effect was estimated for each compound. The developed method can provide at least 80% of results within ±25% limits except for compounds that are degraded in influent. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. An on-spot internal standard addition approach for accurately determining colistin A and colistin B in dried blood spots using ultra high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Tsai, I-Lin; Kuo, Ching-Hua; Sun, Hsin-Yun; Chuang, Yu-Chung; Chepyala, Divyabharathi; Lin, Shu-Wen; Tsai, Yun-Jung

    2017-10-25

    Outbreaks of multidrug-resistant Gram-negative bacterial infections have been reported worldwide. Colistin, an antibiotic with known nephrotoxicity and neurotoxicity, is now being used to treat multidrug-resistant Gram-negative strains. In this study, we applied an on-spot internal standard addition approach coupled with an ultra high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to quantify colistin A and B from dried blood spots (DBSs). Only 15μL of whole blood was required for each sample. An internal standard with the same yield of extraction recoveries as colistin was added to the spot before sample extraction for accurate quantification. Formic acid in water (0.15%) with an equal volume of acetonitrile (50:50v/v) was used as the extraction solution. With the optimized extraction process and LC-MS/MS conditions, colistin A and B could be quantified from a DBS with respective limits of quantification of 0.13 and 0.27μgmL -1 , and the retention times were spot internal standard addition approach which benefited the precision and accuracy. Results showed that DBS sampling coupled with the sensitive LC-MS/MS method has the potential to be an alternative approach for colistin quantification, where the bias of prodrug hydrolysis in liquid samples is decreased. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Validated method for the determination of perfluorinated compounds in placental tissue samples based on a simple extraction procedure followed by ultra-high performance liquid chromatography-tandem mass spectrometry analysis.

    Science.gov (United States)

    Martín, J; Rodríguez-Gómez, R; Zafra-Gómez, A; Alonso, E; Vílchez, J L; Navalón, A

    2016-04-01

    Xenobiotic exposure during pregnancy is inevitable. Determination of perfluorinated compounds (PFCs), chemicals described as environmental contaminants by Public Health Authorities due to their persistence, bioaccumulation and toxicity, is a challenge. In the present work, a method based on a simplified sample treatment involving freeze-drying, solvent extraction and dispersive clean-up of the extracts using C18 sorbents followed by an ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis was developed and validated for the determination of five perfluorinated carboxylic acids (C4-C8) and perfluorooctane sulfonate (PFOS) in placental tissue samples. The most influential parameters affecting the extraction method and clean-up were optimized using Design of Experiments (DOE). The method was validated using matrix-matched calibration. Found limits of detection (LODs) ranged from 0.03 to 2 ng g(-1) and limits of quantification (LOQs) from 0.08 to 6 ng g(-1), while inter- and intra-day variability was under 14% in all cases. Recovery rates for spiked samples ranged from 94% to 113%. The method was satisfactorily applied for the determination of compounds in human placental tissue samples collected at delivery from 25 randomly selected women. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Salting-out assisted liquid-liquid extraction coupled to ultra-high performance liquid chromatography-tandem mass spectrometry for the determination of tetracycline residues in infant foods.

    Science.gov (United States)

    Moreno-González, David; García-Campaña, Ana M

    2017-04-15

    The use of salting-out assisted liquid-liquid extraction (SALLE) combined with ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) has been evaluated for the determination of tetracyclines in infant foods based on meat and vegetables or in milk. To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized. Analytical performances of the method were satisfactory, obtaining limits of quantification lower than 0.48μgkg -1 in all cases. The precision, expressed as relative standard deviation (%, RSD) was below 11.3%. The extraction efficiency for fortified samples ranged from 89.2 to 96.8%, with RSDs lower than 7.3%. Matrix effect was evaluated for all samples studied, being lower than |21|% in all cases. In relation to the low solvent consumption, the proposed methodology could be considered rapid, cheap and environmentally friendly. Its applicability has been successfully tested in a wide range of infant foods. Copyright © 2016 Elsevier Ltd. All rights reserved.

  17. Metabolic profiling of nuciferine in rat urine, plasma, bile and feces after oral administration using ultra-high performance liquid chromatography-diode array detection-quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Wu, Xiao-Lei; Wu, Ming-Jiang; Chen, Xin-Ze; Ma, Hao-Ling; Ding, Li-Qin; Qiu, Feng; Pan, Qin; Zhang, De-Qin

    2017-06-05

    Nuciferine, a major alkaloid found in Nelumbinis Folium, exhibits a broad spectrum of bioactivities, such as antiobesity, anti-diabetes and anti-inflammatory. However, many research regarding nuciferine focused on the extraction, isolation and biological activity, the metabolism is not comprehensively explained in vivo. Thence, the present of this paper is to establish a simple method for speculating metabolites of nuciferine. A total of 15 metabolites were detected and tentatively identified through ultra high performance liquid chromatography-diode array detection-quadrupole time-of-flight mass spectrometry (UHPLC-DAD-QTOF-MS), including 7 new metabolites. Among them, we also discovered a previously unmentioned metabolically active site at the C 1 -OCH 3 position. These metabolites suggested that demethylation, oxidation, glucuronidation and sulfation were major metabolic pathways. This study provided significant experiment basis for its safety estimate and valuable information about the metabolism of nuciferine, which will be advantageous for new drug development. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Short-term toxicity assessments of an antibiotic metabolite in Wistar rats and its metabonomics analysis by ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Han, Hongxing; Xiao, Hailong; Lu, Zhenmei

    2016-02-15

    4-Epi-oxytetracycline (4-EOTC), one of main oxytetracycline (OTC) metabolites, can be commonly detected in food and environment. The toxicity and effects of OTC on animals have been well characterized; however, its metabolites have never been studied systemically. This study aims to investigate 15-day oral dose toxicity and urine metabonomics changes of 4-EOTC after repeated administration in Wistar rats at daily doses of 0.5, 5.0 and 50.0mg/kg bw (bodyweight). Hematology and clinical chemistry parameters, including white blood cell count, red blood cell count, total protein, globulin and albumin/globulin, were obviously altered in rats of 5.0 and 50.0mg/kg bw. Histopathology changes of kidney and liver tissues were also observed in high-dose groups. Urinary metabolites from all groups were analyzed using ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS). Seventeen metabolites contributing to the clusters were identified as potential biomarkers from multivariate analysis, including aminoadipic acid, 6-phosphogluconate, sebacic acid, pipecolic acid, etc. The significant changes of these biomarkers demonstrated metabonomic variations in treated rats, especially lysine and purine metabolism. For the first time in this paper, we combined the results of toxicity and metabonomics induced by 4-EOTC for the serious reconsideration of the safety and potential risks of antibiotics and its degradation metabolites. Copyright © 2016 Elsevier Inc. All rights reserved.

  19. Unbiased Scanning Method and Data Banking Approach Using Ultra-High Performance Liquid Chromatography Coupled with High-Resolution Mass Spectrometry for Quantitative Comparison of Metabolite Exposure in Plasma across Species Analyzed at Different Dates.

    Science.gov (United States)

    Gao, Hongying; Deng, Shibing; Obach, R Scott

    2015-12-01

    An unbiased scanning methodology using ultra high-performance liquid chromatography coupled with high-resolution mass spectrometry was used to bank data and plasma samples for comparing the data generated at different dates. This method was applied to bank the data generated earlier in animal samples and then to compare the exposure to metabolites in animal versus human for safety assessment. With neither authentic standards nor prior knowledge of the identities and structures of metabolites, full scans for precursor ions and all ion fragments (AIF) were employed with a generic gradient LC method to analyze plasma samples at positive and negative polarity, respectively. In a total of 22 tested drugs and metabolites, 21 analytes were detected using this unbiased scanning method except that naproxen was not detected due to low sensitivity at negative polarity and interference at positive polarity; and 4'- or 5-hydroxy diclofenac was not separated by a generic UPLC method. Statistical analysis of the peak area ratios of the analytes versus the internal standard in five repetitive analyses over approximately 1 year demonstrated that the analysis variation was significantly different from sample instability. The confidence limits for comparing the exposure using peak area ratio of metabolites in animal plasma versus human plasma measured over approximately 1 year apart were comparable to the analysis undertaken side by side on the same days. These statistical analysis results showed it was feasible to compare data generated at different dates with neither authentic standards nor prior knowledge of the analytes.

  20. High-throughput ultra high performance liquid chromatography combined with mass spectrometry approach for the rapid analysis and characterization of multiple constituents of the fruit of Acanthopanax senticosus (Rupr. et Maxim.) Harms.

    Science.gov (United States)

    Han, Yue; Zhang, Aihua; Sun, Hui; Zhang, Yingzhi; Meng, Xiangcai; Yan, Guangli; Liu, Liang; Wang, Xijun

    2017-05-01

    Acanthopanax senticosus (Rupr. et Maxim.) Harms, a traditional Chinese medicine, has been widely used to improve the function of skeleton, heart, spleen and kidney. This fruit is rich in nutrients, but the chemical constituents of Acanthopanax senticosus fruit are still unclear. A rapid method based on ultra high performance liquid chromatography with time-of-flight mass spectrometry was developed for the compound analysis of Acanthopanax senticosus fruit in vitro and in vivo. In this study, the Acanthopanax senticosus fruit could significantly increase the weight of immune organs, promote the proliferation of lymphatic T cells, regulate the lymphatic B cell function, and decrease the ability of natural killer cells. A total of 104 compounds of Acanthopanax senticosus fruit including lignans, flavones, triterpenoidsaponins, phenolic acids, and other constituents were identified. Among them, seven chemical compounds were reported for the first time in the Acanthopanax senticosus fruit. Compared with the serum sample of blank and dosed samples, 24 prototype compositions were characterized. The results of our experiment could be helpful to understand the complex compounds of Acanthopanax senticosus fruit in vitro and in vivo for further pharmacological activity studies. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Human exposure assessment to a large set of polymer additives through the analysis of urine by solid phase extraction followed by ultra high performance liquid chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Pouech, Charlène; Kiss, Agneta; Lafay, Florent; Léonard, Didier; Wiest, Laure; Cren-Olivé, Cécile; Vulliet, Emmanuelle

    2015-12-04

    Polymer items are extensively present in the human environment. Humans may be consequently exposed to some compounds, such as additives, incorporated in these items. The objective of this work is to assess the human exposure to the main additives such as those authorized in the packaging for pharmaceutical products. The urinary matrix was selected to optimally answer this challenge because it has already been proven that the exposure to chemicals can be revealed by the analysis of this biological matrix. A multi-residue analytical method for the trace analysis at ng/mL in human urine was developed, and consisted of an extraction of analytes from urine by solid phase extraction (SPE) and an analysis by ultra-high performance liquid chromatography coupled to a tandem mass spectrometer (UHPLC-MS/MS). Even if the quantification of these compounds was an analytical challenge because of (i) the presence of these substances in the analytical process, (ii) the diversity of their physicochemical properties, and (iii) the complexity of the matrix, the optimized method exhibited quantification limits lower than 25ng/mL and recoveries between 51% and 120% for all compounds. The method was validated and applied to 52 human urines. To the best of our knowledge, this work presents the first study allowing the assessment of the occurrence of more than twenty polymer additives at ng/mL in human urine. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. Application of characteristic ion filtering with ultra-high performance liquid chromatography quadrupole time of flight tandem mass spectrometry for rapid detection and identification of chemical profiling in Eucommia ulmoides Oliv.

    Science.gov (United States)

    He, Mingzhen; Jia, Jia; Li, Junmao; Wu, Bei; Huang, Wenping; Liu, Mi; Li, Yan; Yang, Shilin; Ouyang, Hui; Feng, Yulin

    2018-06-15

    Efficient targeted identification of chemical constituents from traditional Chinese medicine is still a major challenge. In this study, we used a characteristic ion filtering strategy to characterize compounds of Eucommia ulmoides Oliv. by ultra-high performance liquid chromatography quadrupole time of flight tandem mass spectrometry (UHPLC-ESI-Q-TOF-MS/MS). By using the ion filtering approach, target constituents of Eucommia ulmoides Oliv. were easily tentatively identified from the enormous LC/MS data set. The strategy consisted of the following three steps: 1) To establishing a characteristic ion database by diagnostic product ions or neutral loss fragments; 2) To evaluate the structural information of the compounds by high-resolution diagnostic characteristic ion filtering; 3) To confirm the different classes by chemical profiling according to their MS/MS spectra. In this study, characteristic ions are summarized as five major groups of compounds in Eucommia ulmoides Oliv. In total, 113 compounds were tentatively identified, including 23 potentially novel compounds. The results form a foundation for the quality control and chemical basis of Eucommia ulmoides Oliv. Copyright © 2018 Elsevier B.V. All rights reserved.

  3. Quantitative determination of multi markers in five varieties of Withania somnifera using ultra-high performance liquid chromatography with hybrid triple quadrupole linear ion trap mass spectrometer combined with multivariate analysis: Application to pharmaceutical dosage forms.

    Science.gov (United States)

    Chandra, Preeti; Kannujia, Rekha; Saxena, Ankita; Srivastava, Mukesh; Bahadur, Lal; Pal, Mahesh; Singh, Bhim Pratap; Kumar Ojha, Sanjeev; Kumar, Brijesh

    2016-09-10

    An ultra-high performance liquid chromatography electrospray ionization tandem mass spectrometry method has been developed and validated for simultaneous quantification of six major bioactive compounds in five varieties of Withania somnifera in various plant parts (leaf, stem and root). The analysis was accomplished on Waters ACQUITY UPLC BEH C18 column with linear gradient elution of water/formic acid (0.1%) and acetonitrile at a flow rate of 0.3mLmin(-1). The proposed method was validated with acceptable linearity (r(2), 0.9989-0.9998), precision (RSD, 0.16-2.01%), stability (RSD, 1.04-1.62%) and recovery (RSD ≤2.45%), under optimum conditions. The method was also successfully applied for the simultaneous determination of six marker compounds in twenty-six marketed formulations. Hierarchical cluster analysis and principal component analysis were applied to discriminate these twenty-six batches based on characteristics of the bioactive compounds. The results indicated that this method is advance, rapid, sensitive and suitable to reveal the quality of Withania somnifera and also capable of performing quality evaluation of polyherbal formulations having similar markers/raw herbs. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Cyclodextrin-based miniaturized solid phase extraction for biopesticides analysis in water and vegetable juices samples analyzed by ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Peng, Li-Qing; Ye, Li-Hong; Cao, Jun; Chang, Yan-Xu; Li, Qin; An, Mingrui; Tan, Zhijing; Xu, Jing-Jing

    2017-07-01

    A cyclodextrin-based miniaturized solid-phase extraction was developed to extract biopesticides from water and vegetable juices. The analytes were detected by ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry. In the solid-phase extraction (SPE) procedure, the liquid sample solution is passed through a packed column filled with 40mg of HP-β-CD, and then the target analytes are absorbed and finally eluted with methanol-acetic acid (90:10, v/v) into a collection tube. The limits of quantification ranged from 3.73 to 16.51ng/mL for a water matrix, from 2.62 to 13.23ng/mL for an orange juice matrix and from 1.76 to 10.35ng/mL for a tomato juice matrix, respectively. The average recovery values were in the range of 88.3-95.9% for the spiked samples. The established methodology was successfully applied to analyze sanguinarine, berberine, rotenone and osthole in water, orange juice and tomato juice. Copyright © 2017 Elsevier Ltd. All rights reserved.

  5. Quantification of Temozolomide in Nonhuman Primate Fluids by Isocratic Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry to Study Brain Tissue Penetration Following Intranasal or Intravenous Delivery

    Directory of Open Access Journals (Sweden)

    Cody J. Peer

    2016-02-01

    Full Text Available A sensitive and selective ultra-high performance liquid chromatography-tandem mass spectrometric method was developed for the quantification of temozolomide (TMZ in nonhuman primate (NHP plasma, cerebrospinal fluid (CSF, and brain extracellular fluid (ECF following microdialysis. Ethyl acetate was used to extract the plasma and CSF samples, using theophylline as the internal standard (IS. ECF samples were diluted with acetonitrile prior to analysis. TMZ was separated on a Waters UPLC® BEH C18 column with an isocratic mobile phase of ammonium acetate (10 mM-0.1% formic acid/acetonitrile (30:70, v/v in a positive-ion multiple reaction monitoring mode (m/z 195.5→137.6 for TMZ; m/z 181.5→124.2 for IS. The retention time of TMZ and theophylline was 0.45 min with a total run time of 2.5 min. The method was validated over the range from 5–2000 ng/mL in NHP plasma, CSF, and ECF with respect to linearity, accuracy, precision, selectivity, and stability. This method was successfully applied toward the measurement of pharmacokinetic samples following various routes of drug administration.

  6. A novel ultra high-performance liquid chromatography-tandem mass spectrometry method for the simultaneous determination of xanthones and steroidal saponins in crude and salt-processed Anemarrhenae Rhizoma aqueous extracts.

    Science.gov (United States)

    Ji, De; Su, Xiaonan; Huang, Ziyan; Wang, Qiaohan; Lu, Tulin

    2018-06-01

    We established a rapid and sensitive ultra high-performance liquid chromatography tandem mass spectrometry method for the simultaneous quantification of xanthones and steroidal saponins in rat plasma. Chromatographic separation was achieved on a C 18 column with a mobile phase comprising acetonitrile and 0.1% formic acid. The detection was performed by negative electrospray ionization in multiple reaction monitoring mode. The validated method showed good linearity within the tested range (r > 0.9945). The intra- and interday precision at high, medium, and low concentrations was less than 7.96%. The bias of accuracies ranged from -1.92 to 9.62%. The extraction recoveries of the compounds ranged from 84.78 to 88.69%, and the matrix effects ranged from 96.76 to 108.59%. This method was successfully applied to a pharmacokinetic comparison of crude and salt-processed Anemarrhenae Rhizoma aqueous extracts after oral administration in rats. The maximum plasma concentration and area under concentration-time curve of timosaponin BIII and timosaponin AIII increased significantly (P < 0.05 or 0.01) and those of timosaponin BII decreased significantly (P < 0.05) after processing. These results could contribute to the clinical application of crude and salt-processed Anemarrhenae Rhizoma and reveal the processing mechanism. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Trace determination of organophosphate esters in white wine, red wine, and beer samples using dispersive liquid-liquid microextraction combined with ultra-high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Pang, Long; Yang, Huiqiang; Yang, Peijie; Zhang, Hongzhong; Zhao, Jihong

    2017-08-15

    In this study, dispersive liquid-liquid microextraction coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry was developed for the analysis of five representative organophosphate esters (OPEs) in wine samples. Under optimized conditions, the proposed method resulted in good linearity (R 2 >0.9933) over the range of 0.1-100μgL -1 , with limits of detection (LODs, S/N =3) and quantification (LOQs, S/N =10) in the ranges of 0.48-18.8ngL -1 and 1.58-62.5ngL -1 , respectively. Inter- and intra-assay precisions of RSD% ranged from 3.21% to 6.13% and from 1.69% to 7.63%, respectively. The spiked recoveries of target OPEs from white wine, red wine, and beer samples were in the ranges of 80-122%, 76-120%, and 76-110%, respectively, at two different concentration levels. The total concentrations of five OPEs found in white wine, red wine, and beer samples were in the ranges of 0.29-0.85μgL -1 , 1.00-3.05μgL -1 , and 0.86-1.47μgL -1 , respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Detection, concentrations and distribution of paxilline, an animal neurotoxin, in mouse brain: an application of ultra-high sensitivity detection of 14C by accelerator mass spectrometry

    International Nuclear Information System (INIS)

    Roberts, P.B.; Kim, K.

    1999-01-01

    Full text: Paxilline is an intermediate in the biosynthesis of lolitrem neurotoxins that cause the disorder rye grass staggers in livestock grazing on pastures infected with certain fungi. Paxilline itself produces similar symptoms and the 14 C-labelled compound has been produced bio-synthetically at low specific activity. Using conventional liquid scintillation counting it was not possible to detect the labelled compound in the brain of mice sacrificed at the time they displayed physiological symptoms. Accelerator mass spectrometry (AMS) counts 14 C atoms, not decays, and provides sensitivity 10,000-100,000 times greater than conventional scintillation counting of radioactive decays. Measurements are easily obtained at the level of the natural abundance of 14 C in living tissue of 6fCi or 10 -16 moles 14 C per mg total carbon. Extraction of the labelled compound from the tissue is unnecessary and sample size can be 0.01-10mg. Paxilline (8mg/kg ip) was given to 25g mice. The total activity injected was 11,000 dpm though the results showed that 1,000dpm would have been sufficient. The concentration of paxilline in homogenised whole brain was determined to be 985 pg or 0.0075 dpm mg dry tissue. The concentration in the major brain segments ranged from 893-1137 pgmg dry tissue. The spinal cord contained 719 pg/mg dry tissue. Our results suggest that toxicologists and pharmacologists should consider what new information may be obtained by combining tracer studies with the power of AMS detection. The AMS method makes possible great reductions in the amount of label and sample sizes, plus wider ranges in concentration/time course studies. In particular, it opens up new possibilities such as: studies at true dietary or environmental levels; tracer studies in large animal or plant systems; field trials; human studies where radiation dose must be considered; and studies with compounds that can only be synthesised with low specific activity. Copyright (1999) Australasian

  9. Simultaneous detection and identification of precursors, degradation and co-products of chemical warfare agents in drinking water by ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Tak, Vijay; Purohit, Ajay; Pardasani, Deepak; Goud, D Raghavender; Jain, Rajeev; Dubey, D K

    2014-11-28

    Environmental markers of chemical warfare agents (CWAs) comprise millions of chemical structures. The simultaneous detection and identification of these environmental markers poses difficulty due to their diverse chemical properties. In this work, by using ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-QTOF), a generic analytical method for the detection and identification of wide range of environmental markers of CWAs (including precursors, degradation and co-products of nerve agents and sesqui-mustards) in drinking water, was developed. The chromatographic analysis of 55 environmental markers of CWAs including isomeric and isobaric compounds was accomplished within 20 min, using 1.8 μm particle size column. Subsequent identification of the compounds was achieved by the accurate mass measurement of either protonated molecule [M+H](+) or ammonium adduct [M+NH4](+) and fragment ions. Isomeric and isobaric compounds were distinguished by chromatographic retention time, characteristic fragment ions generated by both in-source collision induced dissociation (CID) and CID in the collision cell by MS/MS experiments. The exact mass measurement errors for all ions were observed less than 3 ppm with internal calibration. The method limits of detection (LODs) and limits of quantification (LOQs) were determined in drinking water and found to be 1-50 ng mL(-1) and 5-125 ng mL(-1), respectively. Applicability of the proposed method was proved by determining the environmental markers of CWAs in aqueous samples provided by Organization for the Prohibition of Chemical Weapons during 34th official proficiency test. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Zooming into Molecular Biomarker Distribution through Spatially Resolved Mass Spectrometry on Intact Sediment Sections

    Science.gov (United States)

    Wörmer, L.; Fuchser, J.; Alfken, S.; Elvert, M.; Schimmelmann, A.; Hinrichs, K. U.

    2016-02-01

    Marine microorganisms adapt to their habitat by structural modification of their membrane lipids. After sedimentation, and due to their persistence in the sedimentary record, the information archived in them remains available on geological time-scales. Thereby sedimentary lipid biomarkers become important informants of past environments. Conventional biomarker analysis is labor-intensive and requires cm-sized samples, temporal resolution is consequently low. We here present an approach, based on laser desorption ionization (LDI) coupled to ultra high resolution mass spectrometry, that avoids wet-chemical sample preparation and enables analysis directly on sediment sections at sub-mm spatial resolution. Our initial study targeted archaeal glycerol dialkyl glycerol tetraethers (GDGTs). GDGTS are ubiquitous and persistent components in marine sediments, and used in several, widely recognized paleoenvironmental proxies. Applied to an Eastern Mediterranean Sapropel layer, GDGT-profiles with previously unachieved temporal resolution were obtained, and pointed to a strong influence of high frequency cycles on sea-surface temperature and planktonic archaeal ecology. Spatial information furthermore revealed a new view on the fine-scale patchiness of lipid distribution. Following these pioneering studies, major developments are under way. A dedicated facility has been set up at MARUM/University of Bremen, which combines lipid biomarker and elemental analysis at sub-mm resolution (down to 50 µm). We present methods for other comprehensive lipid biomarkers (e.g. alkenones or sterols) that are currently being targeted; and the application of spatially resolved biomarker analysis to recent laminated sediments (Santa Barbara Basin), yielding informative profiles with subannual resolution. We also discuss criteria for analyte and sample selection, as well as the main potentialities and constraints of this new approach.

  11. An improved pseudotargeted metabolomics approach using multiple ion monitoring with time-staggered ion lists based on ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry

    International Nuclear Information System (INIS)

    Wang, Yang; Liu, Fang; Li, Peng; He, Chengwei; Wang, Ruibing; Su, Huanxing; Wan, Jian-Bo

    2016-01-01

    Pseudotargeted metabolomics is a novel strategy integrating the advantages of both untargeted and targeted methods. The conventional pseudotargeted metabolomics required two MS instruments, i.e., ultra-high performance liquid chromatography/quadrupole-time- of-flight mass spectrometry (UHPLC/Q-TOF MS) and UHPLC/triple quadrupole mass spectrometry (UHPLC/QQQ-MS), which makes method transformation inevitable. Furthermore, the picking of ion pairs from thousands of candidates and the swapping of the data between two instruments are the most labor-intensive steps, which greatly limit its application in metabolomic analysis. In the present study, we proposed an improved pseudotargeted metabolomics method that could be achieved on an UHPLC/Q-TOF/MS instrument operated in the multiple ion monitoring (MIM) mode with time-staggered ion lists (tsMIM). Full scan-based untargeted analysis was applied to extract the target ions. After peak alignment and ion fusion, a stepwise ion picking procedure was used to generate the ion lists for subsequent single MIM and tsMIM. The UHPLC/Q-TOF tsMIM MS-based pseudotargeted approach exhibited better repeatability and a wider linear range than the UHPLC/Q-TOF MS-based untargeted metabolomics method. Compared to the single MIM mode, the tsMIM significantly increased the coverage of the metabolites detected. The newly developed method was successfully applied to discover plasma biomarkers for alcohol-induced liver injury in mice, which indicated its practicability and great potential in future metabolomics studies. - Highlights: • An UHPLC/Q-TOF tsMIM MS-based pseudotargeted metabolomics was proposed. • Compared to full scan, the improved method exhibits better repeatability and a wider linear range. • The proposed method could achieve pseudotargeted analysis on one UHPLC/Q-TOF/MS instrument. • The developed method was successfully used to discover biomarkers for alcohol-induced liver injury.

  12. Fast, rugged and sensitive ultra high pressure liquid chromatography tandem mass spectrometry method for analysis of cyanotoxins in raw water and drinking water--First findings of anatoxins, cylindrospermopsins and microcystin variants in Swedish source waters and infiltration ponds.

    Science.gov (United States)

    Pekar, Heidi; Westerberg, Erik; Bruno, Oscar; Lääne, Ants; Persson, Kenneth M; Sundström, L Fredrik; Thim, Anna-Maria

    2016-01-15

    Freshwater blooms of cyanobacteria (blue-green algae) in source waters are generally composed of several different strains with the capability to produce a variety of toxins. The major exposure routes for humans are direct contact with recreational waters and ingestion of drinking water not efficiently treated. The ultra high pressure liquid chromatography tandem mass spectrometry based analytical method presented here allows simultaneous analysis of 22 cyanotoxins from different toxin groups, including anatoxins, cylindrospermopsins, nodularin and microcystins in raw water and drinking water. The use of reference standards enables correct identification of toxins as well as precision of the quantification and due to matrix effects, recovery correction is required. The multi-toxin group method presented here, does not compromise sensitivity, despite the large number of analytes. The limit of quantification was set to 0.1 μg/L for 75% of the cyanotoxins in drinking water and 0.5 μg/L for all cyanotoxins in raw water, which is compliant with the WHO guidance value for microcystin-LR. The matrix effects experienced during analysis were reasonable for most analytes, considering the large volume injected into the mass spectrometer. The time of analysis, including lysing of cell bound toxins, is less than three hours. Furthermore, the method was tested in Swedish source waters and infiltration ponds resulting in evidence of presence of anatoxin, homo-anatoxin, cylindrospermopsin and several variants of microcystins for the first time in Sweden, proving its usefulness. Copyright © 2015 The Authors. Published by Elsevier B.V. All rights reserved.

  13. An improved pseudotargeted metabolomics approach using multiple ion monitoring with time-staggered ion lists based on ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Yang; Liu, Fang; Li, Peng; He, Chengwei; Wang, Ruibing; Su, Huanxing; Wan, Jian-Bo, E-mail: jbwan@umac.mo

    2016-07-13

    Pseudotargeted metabolomics is a novel strategy integrating the advantages of both untargeted and targeted methods. The conventional pseudotargeted metabolomics required two MS instruments, i.e., ultra-high performance liquid chromatography/quadrupole-time- of-flight mass spectrometry (UHPLC/Q-TOF MS) and UHPLC/triple quadrupole mass spectrometry (UHPLC/QQQ-MS), which makes method transformation inevitable. Furthermore, the picking of ion pairs from thousands of candidates and the swapping of the data between two instruments are the most labor-intensive steps, which greatly limit its application in metabolomic analysis. In the present study, we proposed an improved pseudotargeted metabolomics method that could be achieved on an UHPLC/Q-TOF/MS instrument operated in the multiple ion monitoring (MIM) mode with time-staggered ion lists (tsMIM). Full scan-based untargeted analysis was applied to extract the target ions. After peak alignment and ion fusion, a stepwise ion picking procedure was used to generate the ion lists for subsequent single MIM and tsMIM. The UHPLC/Q-TOF tsMIM MS-based pseudotargeted approach exhibited better repeatability and a wider linear range than the UHPLC/Q-TOF MS-based untargeted metabolomics method. Compared to the single MIM mode, the tsMIM significantly increased the coverage of the metabolites detected. The newly developed method was successfully applied to discover plasma biomarkers for alcohol-induced liver injury in mice, which indicated its practicability and great potential in future metabolomics studies. - Highlights: • An UHPLC/Q-TOF tsMIM MS-based pseudotargeted metabolomics was proposed. • Compared to full scan, the improved method exhibits better repeatability and a wider linear range. • The proposed method could achieve pseudotargeted analysis on one UHPLC/Q-TOF/MS instrument. • The developed method was successfully used to discover biomarkers for alcohol-induced liver injury.

  14. Application of ultra-high-performance liquid chromatography coupled with LTQ-Orbitrap mass spectrometry for identification, confirmation and quantitation of illegal adulterated weight-loss drugs in plant dietary supplements.

    Science.gov (United States)

    Cheng, Qiaoyuan; Shou, Linjun; Chen, Cen; Shi, Shi; Zhou, Minghao

    2017-10-01

    In this paper, an ultra-high-performance liquid chromatography coupled with linear ion trap quadrupole Orbitrap high resolution mass spectrometry (UHPLC-LTQ-Orbitrap HRMS) method was developed and validated for identification, confirmation and quantitation of illegal adulterated weight-loss drugs in plant dietary supplements. 13 wt-loss drugs were well separated by the gradient elution of 10mmol/L ammonium acetate - 0.05% formic acid H 2 O and acetonitrile at a flow rate of 0.2mL/min within 12min. The MS analysis was operated under the positive ion and in full MS/dd-MS 2 (data-dependent MS 2 ) mode. The full MS scan with resolution at 60 000 FWHM and narrow mass windows at 5ppm acquired data for identification and quantitation, and dd-MS 2 scan with resolution at 15 000 FWHM obtained product ions for confirmation. The method validation showed good linearity with coefficients of determination (r 2 ) higher than 0.9951 for all analytes. Meantime, all the LOD and LLOQ values were in the respective range of 0.3-2 and 1-9ng/g. The accuracy, intra- and inter-day precision were in the ranges of -1.7 to 3.4%, 1.7-5.0% and 1.9-4.4%, respectively. The mean recoveries ranged from 85.4 to 107.1%, while the absolute and relative matrix effect were in the corresponding range of 98.2-108.6% and 2.6-8.7%. Among 120 batches of weight loss plant dietary supplements, sibutramine and fluoxertine or both were positive in 29 samples. In general, LTQ-Orbitrap HRMS technology was a powerful tool for the analysis of illegal ingredients in dietary supplements. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Identification of Ginkgo biloba supplements adulteration using high performance thin layer chromatography and ultra high performance liquid chromatography-diode array detector-quadrupole time of flight-mass spectrometry.

    Science.gov (United States)

    Avula, Bharathi; Sagi, Satyanarayanaraju; Gafner, Stefan; Upton, Roy; Wang, Yan-Hong; Wang, Mei; Khan, Ikhlas A

    2015-10-01

    Ginkgo biloba is one of the most widely sold herbal supplements and medicines in the world. Its popularity stems from having a positive effect on memory and the circulatory system in clinical studies. As ginkgo popularity increased, non-proprietary extracts were introduced claiming to have a similar phytochemical profile as the clinically tested extracts. The standardized commercial extracts of G. biloba leaf used in ginkgo supplements contain not less than 6% sesquiterpene lactones and 24% flavonol glycosides. While sesquiterpene lactones are unique constituents of ginkgo leaf, the flavonol glycosides are found in many other botanical extracts. Being a high value botanical, low quality ginkgo extracts may be subjected to adulteration with flavonoids to meet the requirement of 24% flavonol glycosides. Chemical analysis by ultra high performance liquid chromatography-mass spectrometry revealed that adulteration of ginkgo leaf extracts in many of these products is common, the naturally flavonol glycoside-rich extract being spiked with pure flavonoids or extracts made from another flavonoid-rich material, such as the fruit/flower of Japanese sophora (Styphnolobium japonicum), which also contains the isoflavone genistein. Recently, genistein has been proposed as an analytical marker for the detection of adulteration of ginkgo extracts with S. japonicum. This study confirms that botanically authenticated G. biloba leaf and extracts made therefrom do not contain genistein, and the presence of which even in trace amounts is suggestive of adulteration. In addition to the mass spectrometric approach, a high performance thin layer chromatography method was developed as a fast and economic method for chemical fingerprint analysis of ginkgo samples.

  16. An improved pseudotargeted metabolomics approach using multiple ion monitoring with time-staggered ion lists based on ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Wang, Yang; Liu, Fang; Li, Peng; He, Chengwei; Wang, Ruibing; Su, Huanxing; Wan, Jian-Bo

    2016-07-13

    Pseudotargeted metabolomics is a novel strategy integrating the advantages of both untargeted and targeted methods. The conventional pseudotargeted metabolomics required two MS instruments, i.e., ultra-high performance liquid chromatography/quadrupole-time- of-flight mass spectrometry (UHPLC/Q-TOF MS) and UHPLC/triple quadrupole mass spectrometry (UHPLC/QQQ-MS), which makes method transformation inevitable. Furthermore, the picking of ion pairs from thousands of candidates and the swapping of the data between two instruments are the most labor-intensive steps, which greatly limit its application in metabolomic analysis. In the present study, we proposed an improved pseudotargeted metabolomics method that could be achieved on an UHPLC/Q-TOF/MS instrument operated in the multiple ion monitoring (MIM) mode with time-staggered ion lists (tsMIM). Full scan-based untargeted analysis was applied to extract the target ions. After peak alignment and ion fusion, a stepwise ion picking procedure was used to generate the ion lists for subsequent single MIM and tsMIM. The UHPLC/Q-TOF tsMIM MS-based pseudotargeted approach exhibited better repeatability and a wider linear range than the UHPLC/Q-TOF MS-based untargeted metabolomics method. Compared to the single MIM mode, the tsMIM significantly increased the coverage of the metabolites detected. The newly developed method was successfully applied to discover plasma biomarkers for alcohol-induced liver injury in mice, which indicated its practicability and great potential in future metabolomics studies. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Ultra high energy gamma-ray astronomy

    International Nuclear Information System (INIS)

    Wdowczyk, J.

    1986-01-01

    The experimental data on ultra high energy γ-rays are reviewed and a comparison of the properties of photon and proton initiated shower is made. The consequences of the existence of the strong ultra high energy γ-ray sources for other observations is analysed and possible mechanisms for the production of ultra high energy γ-rays in the sources are discussed. It is demonstrated that if the γ-rays are produced via cosmic ray interactions the sources have to produce very high fluxes of cosmic ray particles. In fact it is possible that a small number of such sources can supply the whole Galactic cosmic ray flux

  18. Solid-phase extraction in combination with dispersive liquid-liquid microextraction and ultra-high performance liquid chromatography-tandem mass spectrometry analysis: the ultra-trace determination of 10 antibiotics in water samples.

    Science.gov (United States)

    Liang, Ning; Huang, Peiting; Hou, Xiaohong; Li, Zhen; Tao, Lei; Zhao, Longshan

    2016-02-01

    A novel method, solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME), was developed for ultra-preconcentration of 10 antibiotics in different environmental water samples prior to ultra-high performance liquid chromatography-tandem mass spectrometry detection. The optimized results were obtained as follows: after being adjusted to pH 4.0, the water sample was firstly passed through PEP-2 column at 10 mL min(-1), and then methanol was used to elute the target analytes for the following steps. Dichloromethane was selected as extraction solvent, and methanol/acetonitrile (1:1, v/v) as dispersive solvent. Under optimal conditions, the calibration curves were linear in the range of 1-1000 ng mL(-1) (sulfamethoxazole, cefuroxime axetil), 5-1000 ng mL(-1) (tinidazole), 10-1000 ng mL(-1) (chloramphenicol), 2-1000 ng mL(-1) (levofloxacin oxytetracycline, doxycycline, tetracycline, and ciprofloxacin) and 1-400 ng mL(-1) (sulfadiazine) with a good precision. The LOD and LOQ of the method were at very low levels, below 1.67 and 5.57 ng mL(-1), respectively. The relative recoveries of the target analytes were in the range from 64.16% to 99.80% with relative standard deviations between 0.7 and 8.4%. The matrix effect of this method showed a great decrease compared with solid-phase extraction and a significant value of enrichment factor (EF) compared with dispersive liquid-liquid microextraction. The developed method was successfully applied to the extraction and analysis of antibiotics in different water samples with satisfactory results.

  19. A validated analytical method to study the long-term stability of natural and synthetic glucocorticoids in livestock urine using ultra-high performance liquid chromatography coupled to Orbitrap-high resolution mass spectrometry.

    Science.gov (United States)

    De Clercq, Nathalie; Julie, Vanden Bussche; Croubels, Siska; Delahaut, Philippe; Vanhaecke, Lynn

    2013-08-02

    Due to their growth-promoting effects, the use of synthetic glucocorticoids is strictly regulated in the European Union (Council Directive 2003/74/EC). In the frame of the national control plans, which should ensure the absence of residues in food products of animal origin, in recent years, a higher frequency of prednisolone positive bovine urines has been observed. This has raised questions with respect to the stability of natural corticoids in the respective urine samples and their potential to be transformed into synthetic analogs. In this study, a ultra high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS) methodology was developed to examine the stability of glucocorticoids in bovine urine under various storage conditions (up to 20 weeks) and to define suitable conditions for sample handling and storage, using an Orbitrap Exactive™. To this end, an extraction procedure was optimized using a Plackett-Burman experimental design to determine the key conditions for optimal extraction of glucocorticoids from urine. Next, the analytical method was successfully validated according to the guidelines of CD 2002/657/EC. Decision limits and detection capabilities for prednisolone, prednisone and methylprednisolone ranged, respectively, from 0.1 to 0.5μgL(-1) and from 0.3 to 0.8μgL(-1). For the natural glucocorticoids limits of detection and limits of quantification for dihydrocortisone, cortisol and cortisone ranged, respectively, from 0.1 to 0.2μgL(-1) and from 0.3 to 0.8μgL(-1). The stability study demonstrated that filter-sterilization of urine, storage at -80°C, and acidic conditions (pH 3) were optimal for preservation of glucocorticoids in urine and able to significantly limit degradation up to 20 weeks. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Short-term toxicity assessments of an antibiotic metabolite in Wistar rats and its metabonomics analysis by ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry

    International Nuclear Information System (INIS)

    Han, Hongxing; Xiao, Hailong; Lu, Zhenmei

    2016-01-01

    4-Epi-oxytetracycline (4-EOTC), one of main oxytetracycline (OTC) metabolites, can be commonly detected in food and environment. The toxicity and effects of OTC on animals have been well characterized; however, its metabolites have never been studied systemically. This study aims to investigate 15-day oral dose toxicity and urine metabonomics changes of 4-EOTC after repeated administration in Wistar rats at daily doses of 0.5, 5.0 and 50.0 mg/kg bw (bodyweight). Hematology and clinical chemistry parameters, including white blood cell count, red blood cell count, total protein, globulin and albumin/globulin, were obviously altered in rats of 5.0 and 50.0 mg/kg bw. Histopathology changes of kidney and liver tissues were also observed in high-dose groups. Urinary metabolites from all groups were analyzed using ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS). Seventeen metabolites contributing to the clusters were identified as potential biomarkers from multivariate analysis, including aminoadipic acid, 6-phosphogluconate, sebacic acid, pipecolic acid, etc. The significant changes of these biomarkers demonstrated metabonomic variations in treated rats, especially lysine and purine metabolism. For the first time in this paper, we combined the results of toxicity and metabonomics induced by 4-EOTC for the serious reconsideration of the safety and potential risks of antibiotics and its degradation metabolites. - Highlights: • 4-Epioxytetracycline (4-EOTC) induced damages in liver and kidney. • Metabonomics changes especially amino acid and purine metabolism were observed. • Security of OTC metabolite 4-EOTC should be taken into serious reconsideration.

  1. Identification of regioisomers of methylated kaempferol and quercetin by ultra high performance liquid chromatography quadrupole time-of-flight (UHPLC–QTOF) tandem mass spectrometry combined with diagnostic fragmentation pattern analysis

    International Nuclear Information System (INIS)

    Ma, Chengying; Lv, Haipeng; Zhang, Xinzhong; Chen, Zongmao; Shi, Jiang; Lu, Meiling; Lin, Zhi

    2013-01-01

    Highlights: •Found methane elimination is position-specific for methylated flavonols. •Found retro Diels–Alder fragments retained methoxy at original ring of flavonols. •Proposed a diagnostic pattern for discriminating regioisomers of flavonols. •Identified the specificity of three novel flavonol O-methyltransferases. •Identified six biologically active compounds and four new compounds. -- Abstract: The O-methylation of active flavonoids can enhance their antiallergic, anticancerous, and cardioprotective effects depending on the methylation position. Thus, it is biologically and pharmacologically important to differentiate methylated flavonoid regioisomers. In this study, we examined the regioisomers of methylated kaempferol and quercetin using ultra high performance liquid chromatography quadrupole time-of-flight tandem mass spectrometry. The methyl groups on the flavonoids can generally be cleaved as methyl radicals in a position-independent manner. We found that methyl groups can be cleaved as methane. If there are protons adjacent the methoxy on the flavonol rings, intra-molecule proton transfer can occur via collision-induced dissociation, and one molecule of methane can then be eliminated. The remaining charged fragment ([M+H−CH 4 ] + ) reflects the adjacent structure and is specific to the methoxy position. Furthermore, the retro Diels–Alder (RDA) fragmentation of methylated flavonols can generate fragments with the methoxy at the original methylated ring. Combining the position-specific [M+H−CH 4 ] + fragment with the RDA fragments provides a diagnostic pattern for rapidly identifying methylated regioisomeric flavonols. Along with their retention behaviour, we have successfully identified ten regioisomers of methylated kaempferol and quercetin, which include six compounds previously reported in plants and shown to be biologically active. The developed approach is sensitive, rapid, reliable, and requires few standard compounds. It is highly

  2. Screening for in vitro metabolites of kakkalide and irisolidone in human and rat intestinal bacteria by ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Zhang, Guozhe; Gong, Tianxing; Kano, Yoshihiro; Yuan, Dan

    2014-02-01

    Kakkalide and irisolidone, the main isoflavones of Flos Puerariae, exhibit a wide spectrum of bioactivities. Intestinal bacteria biotransformation plays an important role in the metabolic pathways of flavones, and is directly related to the bioactivities of the prodrugs after oral administration. To the best of our knowledge, the metabolic pathways of kakkalide and irisolidone in vitro have not been comprehensively studied yet. This paper describes the strategy using ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UHPLC/Q-TOF MS) for the rapid analysis of the metabolic profiles of kakkalide and irisolidone after incubated with human and rat intestinal bacteria. Bacteria incubated samples were prepared and analyzed after incubated under anaerobic conditions for 48 h. A total of 17 metabolites, including parent compounds, were detected in human and rat intestinal bacteria incubated samples. The results obtained indicate that hydrolysis, dehydroxylation, demethoxylation, demethylation, hydroxylation, decarbonylation, and reduction were the detected metabolic pathways of kakkalide and irisolidone in vitro. The conversion rate of irisolidone in human and rat bacteria was 8.57% and 6.51%, respectively. Biochanin A was the relatively main metabolite of irisolidone, and the content of biochanin A in human and rat bacteria was 3.68% and 4.25%, respectively. The conversion rate of kakkalide in human and rat bacteria was 99.92% and 98.58%, respectively. Irisolidone was the main metabolite of kakkalide, and the content of irisolidone in human and rat bacteria was 89.58% and 89.38%, respectively. This work not only provides the evidence of kakkalide and irisolidone metabolites in vivo, but also demonstrates a simple, fast, sensitive, and inexpensive method for identification of metabolites of other compounds transformed by intestinal bacteria. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. Doping control analysis of 46 polar drugs in horse plasma and urine using a 'dilute-and-shoot' ultra high performance liquid chromatography-high resolution mass spectrometry approach.

    Science.gov (United States)

    Kwok, Wai Him; Choi, Timmy L S; Kwok, Karen Y; Chan, George H M; Wong, Jenny K Y; Wan, Terence S M

    2016-06-17

    The high sensitivity of ultra high performance liquid chromatography coupled with high resolution mass spectrometry (UHPLC-HRMS) allows the identification of many prohibited substances without pre-concentration, leading to the development of simple and fast 'dilute-and-shoot' methods for doping control for human and equine sports. While the detection of polar drugs in plasma and urine is difficult using liquid-liquid or solid-phase extraction as these substances are poorly extracted, the 'dilute-and-shoot' approach is plausible. This paper describes a 'dilute-and-shoot' UHPLC-HRMS screening method to detect 46 polar drugs in equine urine and plasma, including some angiotensin-converting enzyme (ACE) inhibitors, sympathomimetics, anti-epileptics, hemostatics, the new doping agent 5-aminoimidazole-4-carboxamide-1-β-d-ribofuranoside (AICAR), as well as two threshold substances, namely dimethyl sulfoxide and theobromine. For plasma, the sample (200μL) was protein precipitated using trichloroacetic acid, and the resulting supernatant was diluted using Buffer A with an overall dilution factor of 3. For urine, the sample (20μL) was simply diluted 50-fold with Buffer A. The diluted plasma or urine sample was then analysed using a UHPLC-HRMS system in full-scan ESI mode. The assay was validated for qualitative identification purpose. This straightforward and reliable approach carried out in combination with other screening procedures has increased the efficiency of doping control analysis in the laboratory. Moreover, since the UHPLC-HRMS data were acquired in full-scan mode, the method could theoretically accommodate an unlimited number of existing and new doping agents, and would allow a retrospectively search for drugs that have not been targeted at the time of analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. A strategy for comprehensive identification of sequential constituents using ultra-high-performance liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometer, application study on chlorogenic acids in Flos Lonicerae Japonicae.

    Science.gov (United States)

    Zhang, Jia-yu; Wang, Zi-jian; Li, Yun; Liu, Ying; Cai, Wei; Li, Chen; Lu, Jian-qiu; Qiao, Yan-jiang

    2016-01-15

    The analytical methodologies for evaluation of multi-component system in traditional Chinese medicines (TCMs) have been inadequate or unacceptable. As a result, the unclarity of multi-component hinders the sufficient interpretation of their bioactivities. In this paper, an ultra-high-performance liquid chromatography coupled with linear ion trap-Orbitrap (UPLC-LTQ-Orbitrap)-based strategy focused on the comprehensive identification of TCM sequential constituents was developed. The strategy was characterized by molecular design, multiple ion monitoring (MIM), targeted database hits and mass spectral trees similarity filter (MTSF), and even more isomerism discrimination. It was successfully applied in the HRMS data-acquisition and processing of chlorogenic acids (CGAs) in Flos Lonicerae Japonicae (FLJ), and a total of 115 chromatographic peaks attributed to 18 categories were characterized, allowing a comprehensive revelation of CGAs in FLJ for the first time. This demonstrated that MIM based on molecular design could improve the efficiency to trigger MS/MS fragmentation reactions. Targeted database hits and MTSF searching greatly facilitated the processing of extremely large information data. Besides, the introduction of diagnostic product ions (DPIs) discrimination, ClogP analysis, and molecular simulation, raised the efficiency and accuracy to characterize sequential constituents especially position and geometric isomers. In conclusion, the results expanded our understanding on CGAs in FLJ, and the strategy could be exemplary for future research on the comprehensive identification of sequential constituents in TCMs. Meanwhile, it may propose a novel idea for analyzing sequential constituents, and is promising for quality control and evaluation of TCMs. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Development of a highly sensitive methodology for quantitative determination of fexofenadine in a microdose study by multiple injection method using ultra-high performance liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Tanaka, Yukari; Yoshikawa, Yutaka; Yasui, Hiroyuki

    2012-01-01

    An ultra high-sensitivity method for quantifying fexofenadine concentration in rat plasma samples by multiple injection method (MIM) was developed for a microdose study. In this study, MIM involved continuous injections of multiple samples containing the single compound into a column of the ultra-HPLC (UHPLC) system, and then, temporary trapping of the analyte at the column head. This was followed by elution of the compound from the column and detection by mass spectrometer. Fexofenadine, used as a model compound in this study, was extracted from the plasma samples by a protein precipitation method. Chromatographic separation was achieved on a reversed-phase C18 column by using a gradient method with 0.1% formic acid and 0.1% formic acid in acetonitrile as the mobile phase. The analyte was quantified in the positive-ion electrospray ionization mode using selected reaction monitoring. In this study, the analytical time per fexofenadine sample was approximately 2 min according to the UHPLC system. The method exhibited the linear dynamic ranges of 5-5000 pg/mL for fexofenadine in rat plasma. The intra-day precisions were from 3.2 to 8.7% and the accuracy range was 95.2-99.3%. The inter-day precisions and accuracies ranged from 3.5 to 8.4% and from 98.6 to 102.6%, respectively. The validated MIM was successfully applied to a microdose study in the rats that received oral administration of 100 µg/kg fexofenadine. We suggest that this method might be beneficial for the quantification of fexofenadine concentrations in a microdose clinical study.

  6. Screening approach by ultra-high performance liquid chromatography-tandem mass spectrometry for the blood quantification of thirty-four toxic principles of plant origin. Application to forensic toxicology.

    Science.gov (United States)

    Carlier, Jérémy; Guitton, Jérôme; Romeuf, Ludovic; Bévalot, Fabien; Boyer, Baptiste; Fanton, Laurent; Gaillard, Yvan

    2015-01-15

    Plant poisonings have left their mark on history and still cause many deaths, whether intentional or accidental. The means to show toxicological evidence of such poisonings should be implemented with great care. This article presents a technique for measuring thirty-nine toxic principles of plant origin in the blood, covering a large amount of toxins from local or exotic plants: α-lobeline, α-solanine, aconitine, ajmaline, atropine, brucine, cephalomannine, colchicine, convallatoxin, cymarine, cytisine, digitoxin, digoxin, emetine, gelsemine, ibogaine, jervine, kavain, lanatoside C, lupanine, mitragynine, neriifolin, oleandrin, ouabain, paclitaxel, physostigmine, pilocarpine, podophyllotoxin, proscillaridin A, reserpine, retrorsine, ricinine, scopolamine, senecionine, sparteine, strophanthidin, strychnine, veratridine and yohimbine. Analysis was carried out using an original ultra-high performance liquid chromatography separation coupled with tandem mass spectrometry detection. Extraction was a standard solid phase extraction performed on Oasis(®) HLB cartridge. Thirty-four of the thirty-nine compounds were put through a validation procedure. The assay was linear in the calibration curve range from 0.5 or 5 μg/L to 1000 μg/L according to the compounds. The method is sensitive (LOD from 0.1 to 1.6 μg/L). The within-day precision of the assay was less than 22.5% at the LLOQ, and the between-day precision was less than 21.5% for 10 μg/L for all the compounds included. The assay accuracy was in the range of 87.4 to 119.8% for the LLOQ. The extraction recovery and matrix effect ranged from 30 to 106% and from -30 to 14%, respectively. It has proven useful and effective in several difficult forensic cases. Copyright © 2014 Elsevier B.V. All rights reserved.

  7. Simultaneous determination of notoginsenoside R₁, ginsenoside Rg₁, ginsenoside Re and 20(S) protopanaxatriol in beagle dog plasma by ultra high performance liquid mass spectrometry after oral administration of a Panax notoginseng saponin preparation.

    Science.gov (United States)

    Wu, Huichao; Liu, Huimin; Bai, Jie; Lu, Yang; Du, Shouying

    2015-01-01

    20(S) protopanaxatriol is the main metabolite of notoginsenoside R1, ginsenoside Rg1, ginsenoside Re in Panax notoginseng and has significant activities. A ultra high performance liquid mass spectrometry method has been developed and validated for the simultaneous determination of notoginsenoside R₁ (R1), ginsenoside Rg₁ (Rg₁), ginsenoside Re (Re) and 20(S) protopanaxatriol (PPT) in beagle dog plasma after oral administration of a Panax notoginseng saponin preparation. After the addition of the internal standard (digoxin), plasma samples were subjected to liquid-liquid extraction with acetone and methanol and separated on a 100 × 2.1 mm ACQUITY 1.7 μm C₁₈ column (Waters, USA), with acetonitrile and water as the mobile phase, within a runtime of 7.0 min. The analytes were detected without interference in Selected Reaction Monitoring mode with a change in the electrospray ionization from positive to negative. The detection limits were 0.01 to 0.04 mg/L and the calibration curves of the peak areas for the four ingredients were linear over four orders of magnitude with a correlation coefficient greater than 0.9957. The intra-day and inter-day precision values (relative standard deviation, RSD, %) were within 10.25% and 13.51%, respectively, and the accuracy (relative error, RE, %) was less than 7.81%. The validated method was successfully applied to a comparative pharmacokinetic study of four saponins in beagle dogs after oral administration of a Panax Notoginseng Saponins preparation. The pharmacokinetic parameters were calculated with DAS 3.20. The Tmax and Cmax values indicate a dose-dose relationship between the saponins (R1, Rg1, and Re) and their sapogenin (PPT). Copyright © 2014 Elsevier B.V. All rights reserved.

  8. The Application of Ultra-High-Performance Liquid Chromatography Coupled with a LTQ-Orbitrap Mass Technique to Reveal the Dynamic Accumulation of Secondary Metabolites in Licorice under ABA Stress.

    Science.gov (United States)

    Li, Da; Xu, Guojie; Ren, Guangxi; Sun, Yufeng; Huang, Ying; Liu, Chunsheng

    2017-10-20

    The traditional medicine licorice is the most widely consumed herbal product in the world. Although much research work on studying the changes in the active compounds of licorice has been reported, there are still many areas, such as the dynamic accumulation of secondary metabolites in licorice, that need to be further studied. In this study, the secondary metabolites from licorice under two different methods of stress were investigated by ultra-high-performance liquid chromatography coupled with hybrid linear ion trap-Orbitrap mass spectrometry (UHPLC-LTQ-Orbitrap-MS). A complex continuous coordination of flavonoids and triterpenoids in a network was modulated by different methods of stress during growth. The results showed that a total of 51 secondary metabolites were identified in licorice under ABA stress. The partial least squares-discriminate analysis (PLS-DA) revealed the distinction of obvious compounds among stress-specific districts relative to ABA stress. The targeted results showed that there were significant differences in the accumulation patterns of the deeply targeted 41 flavonoids and 10 triterpenoids compounds by PCA and PLS-DA analyses. To survey the effects of flavonoid and triterpenoid metabolism under ABA stress, we inspected the stress-specific metabolic changes. Our study testified that the majority of flavonoids and triterpenoids were elevated in licorice under ABA stress, while the signature metabolite affecting the dynamic accumulation of secondary metabolites was detected. Taken together, our results suggest that ABA-specific metabolite profiling dynamically changed in terms of the biosynthesis of flavonoids and triterpenoids, which may offer new trains of thought on the regular pattern of dynamic accumulation of secondary metabolites in licorice at the metabolite level. Our results also provide a reference for clinical applications and directional planting and licorice breeding.

  9. The Application of Ultra-High-Performance Liquid Chromatography Coupled with a LTQ-Orbitrap Mass Technique to Reveal the Dynamic Accumulation of Secondary Metabolites in Licorice under ABA Stress

    Directory of Open Access Journals (Sweden)

    Da Li

    2017-10-01

    Full Text Available The traditional medicine licorice is the most widely consumed herbal product in the world. Although much research work on studying the changes in the active compounds of licorice has been reported, there are still many areas, such as the dynamic accumulation of secondary metabolites in licorice, that need to be further studied. In this study, the secondary metabolites from licorice under two different methods of stress were investigated by ultra-high-performance liquid chromatography coupled with hybrid linear ion trap–Orbitrap mass spectrometry (UHPLC-LTQ-Orbitrap-MS. A complex continuous coordination of flavonoids and triterpenoids in a network was modulated by different methods of stress during growth. The results showed that a total of 51 secondary metabolites were identified in licorice under ABA stress. The partial least squares–discriminate analysis (PLS-DA revealed the distinction of obvious compounds among stress-specific districts relative to ABA stress. The targeted results showed that there were significant differences in the accumulation patterns of the deeply targeted 41 flavonoids and 10 triterpenoids compounds by PCA and PLS-DA analyses. To survey the effects of flavonoid and triterpenoid metabolism under ABA stress, we inspected the stress-specific metabolic changes. Our study testified that the majority of flavonoids and triterpenoids were elevated in licorice under ABA stress, while the signature metabolite affecting the dynamic accumulation of secondary metabolites was detected. Taken together, our results suggest that ABA-specific metabolite profiling dynamically changed in terms of the biosynthesis of flavonoids and triterpenoids, which may offer new trains of thought on the regular pattern of dynamic accumulation of secondary metabolites in licorice at the metabolite level. Our results also provide a reference for clinical applications and directional planting and licorice breeding.

  10. Application of a hybrid ordered mesoporous silica as sorbent for solid-phase multi-residue extraction of veterinary drugs in meat by ultra-high-performance liquid chromatography coupled to ion-trap tandem mass spectrometry.

    Science.gov (United States)

    Casado, Natalia; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Sierra, Isabel

    2016-08-12

    A quick, sensitive and selective analytical reversed-phase multi-residue method using ultra-high performance liquid chromatography coupled to an ion-trap mass spectrometry detector (UHPLC-IT-MS/MS) operating in both positive and negative ion mode was developed for the simultaneous determination of 23 veterinary drug residues (β-blockers, β-agonists and Non-Steroidal Anti-inflammatory Drugs (NSAIDs)) in meat samples. The sample treatment involved a liquid-solid extraction followed by a solid-phase extraction (SPE) procedure. SBA-15 type mesoporous silica was synthetized and modified with octadecylsilane, and the resulting hybrid material (denoted as SBA-15-C18) was applied and evaluated as SPE sorbent in the purification of samples. The materials were comprehensively characterized, and they showed a high surface area, high pore volume and a homogeneous distribution of the pores. Chromatographic conditions and extraction procedure were optimized, and the method was validated according to the Commission Decision 2002/657/EC. The method detection limits (MDLs) and the method quantification limits (MQLs) were determined for all the analytes in meat samples and found to range between 0.01-18.75μg/kg and 0.02-62.50μg/kg, respectively. Recoveries for 15 of the target analytes ranged from 71 to 98%. In addition, for comparative purpose SBA-15-C18 was evaluated towards commercial C18 amorphous silica. Results revealed that SBA-15-C18 was clearly more successful in the multi-residue extraction of the 23 mentioned analytes with higher recovery values. The method was successfully tested to analyze prepacked preparations of mince bovine meat. Traces of propranolol, ketoprofen and diclofenac were detected in some samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Application of Ultra-High-Performance Liquid Chromatography Coupled with LTQ-Orbitrap Mass Spectrometry for the Qualitative and Quantitative Analysis of Polygonum multiflorum Thumb. and Its Processed Products

    Directory of Open Access Journals (Sweden)

    Teng-Hua Wang

    2015-12-01

    Full Text Available In order to quickly and simultaneously obtain the chemical profiles and control the quality of the root of Polygonum multiflorum Thumb. and its processed form, a rapid qualitative and quantitative method, using ultra-high-performance liquid chromatography coupled with electrospray ionization-linear ion trap-Orbitrap hybrid mass spectrometry (UHPLC-LTQ-Orbitrap MSn has been developed. The analysis was performed within 10 min on an AcQuity UPLC™ BEH C18 column with a gradient elution of 0.1% formic acid-acetonitrile at flow rate of 400 μL/min. According to the fragmentation mechanism and high resolution MSn data, a diagnostic ion searching strategy was used for rapid and tentative identification of main phenolic components and 23 compounds were simultaneously identified or tentatively characterized. The difference in chemical profiles between P. multiflorum and its processed preparation were observed by comparing the ions abundances of main constituents in the MS spectra and significant changes of eight metabolite biomarkers were detected in the P. multiflorum samples and their preparations. In addition, four of the representative phenols, namely gallic acid, trans-2,3,5,4′-tetra-hydroxystilbene-2-O-β-d-glucopyranoside, emodin and emodin-8-O-β-d-glucopyranoside were quantified by the validated UHPLC-MS/MS method. These phenols are considered to be major bioactive constituents in P. multiflorum, and are generally regarded as the index for quality assessment of this herb. The method was successfully used to quantify 10 batches of P. multiflorum and 10 batches of processed P. multiflorum. The results demonstrated that the method is simple, rapid, and suitable for the discrimination and quality control of this traditional Chinese herb.

  12. Ultra-high performance liquid chromatography coupled with quadrupole/time of flight mass spectrometry based chemical profiling approach for the holistic quality control of complex Kang-Jing formula preparations.

    Science.gov (United States)

    Yang, Xiao-Huan; Cheng, Xiao-Lan; Qin, Bing; Cai, Zhuo-Ya; Cai, Xiong; Liu, Shao; Wang, Qi; Qin, Yong

    2016-05-30

    The Kang-Jing (KJ) formula is a compound preparation made from 12 kinds of herbs. So far, four different methods (M1-M4) have been documented for KJ preparation, but the influence of preparation methods on the holistic quality of KJ have remained unknown. In this study, a strategy was proposed to investigate the influence of different preparation methods on the holistic quality of KJ using ultra-high performance liquid chromatography coupled with quadrupole/time of flight mass spectrometry (UHPLC-QTOF-MS/MS) based chemical profiling. A total of 101 compounds mainly belonging to flavonoids, tanshinones, monoterpene glycosides, triterpenoid saponins, alkaloids, phenolic acids and volatile oils, were identified. Among these compounds, glaucine was detected only in M3/M4 samples, while two dehydrocorydaline isomers merely detected in M2/M3/M4 samples. Tetrahydrocolumbamine, ethylic lithospermic acid, salvianolic acid E and rosmarimic acid were only detected in M1/M3/M4 samples. In the subsequent quantitative analysis, 12 major compounds were determined by UHPLC-MS/MS. The proposed method was validated with respect to linearity, accuracy, precision and recovery. It was found that the contents of marker compounds varied significantly in samples prepared by different methods. These results demonstrated that preparation method does significantly affect the holistic quality of KJ. UHPLC-QTOF-MS/MS based chemical profiling approach is efficient and reliable for comprehensive quality evaluation of KJ. Collectively, this study provide the chemical evidence for revealing the material basis of KJ, and establish a simple and accurate chemical profiling method for its quality control. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Simultaneous analysis of gemfibrozil, morphine, and its two active metabolites in different mouse brain structures using solid-phase extraction with ultra-high performance liquid chromatography and tandem mass spectrometry with a deuterated internal standard.

    Science.gov (United States)

    Yang, Zizhao; Wang, Lu; Xu, Mingcheng; Gu, Jingkai; Yu, Lushan; Zeng, Su

    2016-06-01

    A rapid and sensitive bioassay was established and validated to simultaneously determine gemfibrozil, morphine, morphine-3β-glucuronide, and morphine-6β-glucuronide in mouse cerebrum, epencephalon, and hippocampus based on ultra-high performance liquid chromatography and tandem mass spectrometry. The deuterated internal standard, M6G-d3, was mixed with the prepared samples at 10 ng/mL as the final concentration. The samples were transferred into the C18 solid-phase extraction columns with gradient elution for solid-phase extraction. The mobile phase consisted of methanol and 0.05% formic acid (pH 3.2). Multiple reaction monitoring has been applied to analyze gemfibrozil (m/z 249.0 → 121.0) in anion mode, and M6G-d3 (m/z 465.1 → 289.1), morphine (m/z 286.0 → 200.9), and M3G and M6G (m/z 462.1 → 286.1) in the positive ion mode. The method has a linear calibration range from 0.05 to 10 ng for gemfibrozil, morphine, and M3G and M6G with correlation coefficients >0.993. The lower limit of quantitation for all four analytes was 0.05 ng/mL, relative standard deviation of intra- and interday precision was less than 10.5%, and the relative error of accuracy was from -8.2 to 8.3% at low, medium, and high concentrations for all the analytes. In conclusion, gemfibrozil can influence the morphine antinociception after coronary heart disease induced chronic angina by the change in one of morphine metabolites', M3G, distribution in mouse brain. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Short-term toxicity assessments of an antibiotic metabolite in Wistar rats and its metabonomics analysis by ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Han, Hongxing [College of Life Sciences, Zhejiang University, 866 Yuhangtang Road, Hangzhou 310058 (China); Xiao, Hailong [Hangzhou Institute for Food and Drug Control, Hangzhou 310004 (China); Lu, Zhenmei, E-mail: lzhenmei@zju.edu.cn [College of Life Sciences, Zhejiang University, 866 Yuhangtang Road, Hangzhou 310058 (China)

    2016-02-15

    4-Epi-oxytetracycline (4-EOTC), one of main oxytetracycline (OTC) metabolites, can be commonly detected in food and environment. The toxicity and effects of OTC on animals have been well characterized; however, its metabolites have never been studied systemically. This study aims to investigate 15-day oral dose toxicity and urine metabonomics changes of 4-EOTC after repeated administration in Wistar rats at daily doses of 0.5, 5.0 and 50.0 mg/kg bw (bodyweight). Hematology and clinical chemistry parameters, including white blood cell count, red blood cell count, total protein, globulin and albumin/globulin, were obviously altered in rats of 5.0 and 50.0 mg/kg bw. Histopathology changes of kidney and liver tissues were also observed in high-dose groups. Urinary metabolites from all groups were analyzed using ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS). Seventeen metabolites contributing to the clusters were identified as potential biomarkers from multivariate analysis, including aminoadipic acid, 6-phosphogluconate, sebacic acid, pipecolic acid, etc. The significant changes of these biomarkers demonstrated metabonomic variations in treated rats, especially lysine and purine metabolism. For the first time in this paper, we combined the results of toxicity and metabonomics induced by 4-EOTC for the serious reconsideration of the safety and potential risks of antibiotics and its degradation metabolites. - Highlights: • 4-Epioxytetracycline (4-EOTC) induced damages in liver and kidney. • Metabonomics changes especially amino acid and purine metabolism were observed. • Security of OTC metabolite 4-EOTC should be taken into serious reconsideration.

  15. Comparative analysis of main bio-active components in the herb pair Danshen-Honghua and its single herbs by ultra-high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry.

    Science.gov (United States)

    Qu, Cheng; Pu, Zong-Jin; Zhou, Gui-Sheng; Wang, Jun; Zhu, Zhen-Hua; Yue, Shi-Jun; Li, Jian-Ping; Shang, Li-Li; Tang, Yu-Ping; Shi, Xu-Qin; Liu, Pei; Guo, Jian-Ming; Sun, Jing; Tang, Zhi-Shu; Zhao, Jing; Zhao, Bu-Chang; Duan, Jin-Ao

    2017-09-01

    A sensitive, reliable, and powerful ultra-high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry method was developed for simultaneous quantification of the 15 main bio-active components including phenolic acids and flavonoids within 13 min for the first time. The proposed method was first reported and validated by good linearity (r 2  > 0.9975), limit of detection (1.12-7.01 ng/mL), limit of quantification (3.73-23.37 ng/mL), intra- and inter-day precisions (RSD ≤ 1.92%, RSD ≤ 2.45%), stability (RSD ≤ 5.63%), repeatability (RSD ≤ 4.34%), recovery (96.84-102.12%), and matrix effects (0.92-1.02). The established analytical methodology was successfully applied to comparative analysis of main bio-active components in the herb pair Danshen-Honghua and its single herbs. Compared to the single herb, the content of most flavonoid glycosides was remarkably increased in their herb pair, and main phenolic acids were decreased, conversely. The content changes of the main components in the herb pair supported the synergistic effects on promoting blood circulation and removing blood stasis. The results provide a scientific basis and reference for the quality control of Danshen-Honghua herb pair and the drug interactions based on variation of bio-active components in herb pairs. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Fast determination of alkylphenol ethoxylates in leafy vegetables using a modified quick, easy, cheap, effective, rugged, and safe method and ultra-high performance supercritical fluid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Jiang, Ze-Jun; Cao, Xiao-Lin; Li, Hui; Zhang, Chan; Abd El-Aty, A M; Jin, Fen; Shao, Hua; Jin, Mao-Jun; Wang, Shan-Shan; She, Yong-Xin; Wang, Jing

    2017-11-24

    In the present study, a quick and sensitive method was developed for simultaneous determination of nonylphenol ethoxylates (NPxEOs) and octylphenol ethoxylates (OPxEOs) (x=2-20) in three leafy vegetables, including cabbage, lettuce, and spinach using a modified "QuEChERS" method and ultra-high performance supercritical fluid chromatography-tandem mass spectrometry (UHPSFC-MS/MS) with scheduled multiple reaction monitoring (MRM). Under optimized conditions, the 38 target analytes were analyzed within a short period of time (5 min). The linearities of the matrix-matched standard calibrations were satisfactory with coefficients of determination (R 2 )>0.99 and the limits of detection (LOD) and quantification (LOQ) were in between 0.02-0.27 and 0.18-1.75μgkg -1 , respectively. The recovery of all target analytes spiked at three (low, medium, and high) fortification levels in various leafy vegetables were ranged from 72.8-122.6% with relative standard deviation (RSD) ≤18.3%. The method was successfully applied to market samples and the target analytes were found in all monitored samples, with total concentrations of 0-8.67μgkg -1 and 15.75-95.75μgkg -1 for OPxEOs and NPxEOs (x=2-20), respectively. In conclusion, the newly developed UHPSFC-ESI-MS/MS method is rapid and versatile and could be extrapolated for qualitative and quantitative analysis of APxEOs in other leafy vegetables. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Ultra-high temperature direct propulsion

    International Nuclear Information System (INIS)

    Araj, K.J.; Slovik, G.; Powell, J.R.; Ludewig, H.

    1987-01-01

    Potential advantages of ultra-high exhaust temperature (3000 K - 4000 K) direct propulsion nuclear rockets are explored. Modifications to the Particle Bed Reactor (PBR) to achieve these temperatures are described. Benefits of ultra-high temperature propulsion are discussed for two missions - orbit transfer (ΔV = 5546 m/s) and interplanetary exploration (ΔV = 20000 m/s). For such missions ultra-high temperatures appear to be worth the additional complexity. Thrust levels are reduced substantially for a given power level, due to the higher enthalpy caused by partial disassociation of the hydrogen propellant. Though technically challenging, it appears potentially feasible to achieve such ultra high temperatures using the PBR

  18. RESOLVING THE LUMINOSITY PROBLEM IN LOW-MASS STAR FORMATION

    Energy Technology Data Exchange (ETDEWEB)

    Dunham, Michael M. [Department of Astronomy, Yale University, P.O. Box 208101, New Haven, CT 06520 (United States); Vorobyov, Eduard I., E-mail: michael.dunham@yale.edu, E-mail: eduard.vorobiev@univie.ac.at [Institute of Astronomy, University of Vienna, Vienna 1180 (Austria)

    2012-03-01

    We determine the observational signatures of protostellar cores by coupling two-dimensional radiative transfer calculations with numerical hydrodynamical simulations that predict accretion rates that both decline with time and feature short-term variability and episodic bursts caused by disk gravitational instability and fragmentation. We calculate the radiative transfer of the collapsing cores throughout the full duration of the collapse, using as inputs the core, disk, protostellar masses, radii, and mass accretion rates predicted by the hydrodynamical simulations. From the resulting spectral energy distributions, we calculate standard observational signatures (L{sub bol}, T{sub bol}, L{sub bol}/L{sub smm}) to directly compare to observations. We show that the accretion process predicted by these models reproduces the full spread of observed protostars in both L{sub bol}-T{sub bol} and L{sub bol}-M{sub core} space, including very low luminosity objects, provides a reasonable match to the observed protostellar luminosity distribution, and resolves the long-standing luminosity problem. These models predict an embedded phase duration shorter than recent observationally determined estimates (0.12 Myr versus 0.44 Myr), and a fraction of total time spent in Stage 0 of 23%, consistent with the range of values determined by observations. On average, the models spend 1.3% of their total time in accretion bursts, during which 5.3% of the final stellar mass accretes, with maximum values being 11.8% and 35.5% for the total time and accreted stellar mass, respectively. Time-averaged models that filter out the accretion variability and bursts do not provide as good of a match to the observed luminosity problem, suggesting that the bursts are required.

  19. Ultra-high-resolution alpha spectrometry for nuclear forensics and safeguards applications

    International Nuclear Information System (INIS)

    Bacrania, Minesh K.; Croce, Mark; Bond, Evelyn; Dry, Donald; Moody, W. Allen; Lamont, Stephen; Rabin, Michael; Rim, Jung; Smith, Audrey; Beall, James; Bennett, Douglas; Kotsubo, Vincent; Horansky, Robert; Hilton, Gene; Schmidt, Daniel; Ullom, Joel; Cantor, Robin

    2010-01-01

    We will present our work on the development of ultra-high-resolution detectors for alpha particle spectrometry. These detectors, based on superconducting transition-edge sensors, offer energy resolution that is five to ten times better than conventional silicon detectors. Using these microcalorimeter detectors, the isotopic composition of mixed-actinide samples can be determined rapidly without the need for actinide separation chemistry to isolate each element, or mass spectrometry to separate isotopic signatures that can not be resolved using traditional alpha spectrometry (e.g. Pu-239/Pu-240, or Pu-238/Am-241). This paper will cover the detector and measurement system, actinide source preparation, and the quantitative isotopic analysis of a number of forensics- and safeguards-relevant radioactive sources.

  20. Selection and evaluation of an ultra high vacuum gate valve for Isabelle beam line vacuum system

    International Nuclear Information System (INIS)

    Foerster, C.L.; McCafferty, D.

    1980-01-01

    A minimum of eighty-four (84) Ultra High Vacuum Gate Valves will be utilized in ISABELLE to protect proton beam lines from catastrophic vacuum failure and to provide sector isolation for maintenance requirements. The valve to be selected must function at less than 1 x 10 -11 Torr pressure and be bakeable to 300 0 C in its open or closed position. In the open position, the valve must have an RF shield to make the beam line walls appear continuous. Several proposed designs were built and evaluated. The evaluation consisted mainly of leak testing, life tests, thermal cycling, mass spectrometer analysis, and 10 -12 Torr operation. Problems with initial design and fabrication were resolved. Special requirements for design and construction were developed. This paper describes the tests on two final prototypes which appear to be the best candidates for ISABELLE operation

  1. Fast determination of pesticides and other contaminants of emerging concern in treated wastewater using direct injection coupled to highly sensitive ultra-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Campos-Mañas, Marina Celia; Plaza-Bolaños, Patricia; Sánchez-Pérez, José Antonio; Malato, Sixto; Agüera, Ana

    2017-07-21

    It is well known that wastewater treatment plant (WWTP) effluents usually contain micropollutants such as pharmaceuticals (or their transformation products, TPs) or pesticides, which is a major issue when evaluating their possible reuse (e.g. for irrigation in agriculture). In search for an improved accuracy and simplicity, methods based on the direct injection of the sample (DI) represent a recent trend taking advantage of the increasing sensitivity of new mass spectrometry (MS) instruments. Thus, the present study shows the development and validation of a DI-based method by ultra-high-performance liquid chromatography quadrupole-linear ion trap analyser (UHPLC-QqLIT-MS/MS). The proposed method was applied to the monitoring of 115 organic microcontaminants (including pharmaceuticals, TPs and pesticides) at the ngL -1 /μgL -1 level in wastewater effluents from urban WWTPs. Sample pre-treatment was reduced to acetonitrile addition and filtration of the mixture previous to LC-MS analysis. Total analysis time was <15min. A subsequent validation protocol was carried out in treated WW (TWW), following indications of SANTE and Eurachem Guidelines. Linearity and matrix effect were evaluated in the range of 10-1000ngL -1 . 70% of the analytes showed a moderate matrix effect (≤25%). Trueness (expressed as recovery) and precision (calculated as relative standard deviation, RSD) were evaluated at four concentration levels (20, 50, 500 and 1000ngL -1 ) in TWW samples. The LODs ranged from 1 to 357ngL -1 and the LOQs from 10 to 500ngL -1 . 92% of the compounds showed limits of quantification ≤100ngL -1 . In most cases, mean recoveries were in the range 70-120%, and RSD values were ≤20%. The validated method was successfully applied to the analysis of 10 TWW samples, demonstrating the occurrence of 67 target compounds at concentration levels from 26705ngL -1 (4-aminoantipyrine) to 10ngL -1 (tebuconazole and bezafibrate). Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Comprehensive profiling of mercapturic acid metabolites from dietary acrylamide as short-term exposure biomarkers for evaluation of toxicokinetics in rats and daily internal exposure in humans using isotope dilution ultra-high performance liquid chromatography tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yu [Department of Food Science and Nutrition, College of Biosystems Engineering and Food Science, Zhejiang University, Hangzhou 310058, Zhejiang (China); Zhejiang Key Laboratory for Agro-Food Processing, Zhejiang R & D Center for Food Technology and Equipment, Fuli Institute of Food Science, Zhejiang University, Hangzhou 310058, Zhejiang (China); Wang, Qiao; Cheng, Jun [Department of Food Science and Nutrition, College of Biosystems Engineering and Food Science, Zhejiang University, Hangzhou 310058, Zhejiang (China); Zhang, Jingshun; Xu, Jiaojiao [Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051, Zhejiang (China); Ren, Yiping, E-mail: renyiping@263.net [Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051, Zhejiang (China)

    2015-09-24

    Mercapturic acid metabolites from dietary acrylamide are important short-term exposure biomarkers for evaluating the in vivo toxicity of acrylamide. Most of studies have focused on the measurement of two metabolites, N-acetyl-S-(2-carbamoylethyl)-L-cysteine (AAMA) and N-acetyl-S-(2-carbamoyl-2-hydroxyethyl)-L-cysteine (GAMA). Thus, the comprehensive profile of acrylamide urinary metabolites cannot be fully understood. We developed an isotope dilution ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method for the simultaneous determination of all four mercapturic acid adducts of acrylamide and its primary metabolite glycidamide under the electroscopy ionization negative (ESI-) mode in the present study. The limit of detection (LOD) and limit of quantification (LOQ) of the analytes ranged 0.1–0.3 ng/mL and 0.4–1.0 ng/mL, respectively. The recovery rates with low, intermediate and high spiking levels were calculated as 95.5%–105.4%, 98.2%–114.0% and 92.2%–108.9%, respectively. Acceptable within-laboratory reproducibility (RSD < 7.0%) substantially supported the use of current method for robust analysis. Rapid pretreatment procedures and short run time (8 min per sample) ensured good efficiency of metabolism profiling, indicating a wide application for investigating short-term internal exposure of dietary acrylamide. Our proposed UHPLC-MS/MS method was successfully applied to the toxicokinetic study of acrylamide in rats. Meanwhile, results of human urine analysis indicated that the levels of N-acetyl-S-(2-carbamoylethyl)-L-cysteine-sulfoxide (AAMA-sul), which did not appear in the mercapturic acid metabolites in rodents, were more than the sum of GAMA and N-acetyl-S-(1-carbamoyl-2-hydroxyethyl)-L-cysteine (iso-GAMA). Thus, AAMA-sul may alternatively become a specific biomarker for investigating the acrylamide exposure in humans. Current proposed method provides a substantial methodology support for comprehensive

  3. Comprehensive profiling of mercapturic acid metabolites from dietary acrylamide as short-term exposure biomarkers for evaluation of toxicokinetics in rats and daily internal exposure in humans using isotope dilution ultra-high performance liquid chromatography tandem mass spectrometry

    International Nuclear Information System (INIS)

    Zhang, Yu; Wang, Qiao; Cheng, Jun; Zhang, Jingshun; Xu, Jiaojiao; Ren, Yiping

    2015-01-01

    Mercapturic acid metabolites from dietary acrylamide are important short-term exposure biomarkers for evaluating the in vivo toxicity of acrylamide. Most of studies have focused on the measurement of two metabolites, N-acetyl-S-(2-carbamoylethyl)-L-cysteine (AAMA) and N-acetyl-S-(2-carbamoyl-2-hydroxyethyl)-L-cysteine (GAMA). Thus, the comprehensive profile of acrylamide urinary metabolites cannot be fully understood. We developed an isotope dilution ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method for the simultaneous determination of all four mercapturic acid adducts of acrylamide and its primary metabolite glycidamide under the electroscopy ionization negative (ESI-) mode in the present study. The limit of detection (LOD) and limit of quantification (LOQ) of the analytes ranged 0.1–0.3 ng/mL and 0.4–1.0 ng/mL, respectively. The recovery rates with low, intermediate and high spiking levels were calculated as 95.5%–105.4%, 98.2%–114.0% and 92.2%–108.9%, respectively. Acceptable within-laboratory reproducibility (RSD < 7.0%) substantially supported the use of current method for robust analysis. Rapid pretreatment procedures and short run time (8 min per sample) ensured good efficiency of metabolism profiling, indicating a wide application for investigating short-term internal exposure of dietary acrylamide. Our proposed UHPLC-MS/MS method was successfully applied to the toxicokinetic study of acrylamide in rats. Meanwhile, results of human urine analysis indicated that the levels of N-acetyl-S-(2-carbamoylethyl)-L-cysteine-sulfoxide (AAMA-sul), which did not appear in the mercapturic acid metabolites in rodents, were more than the sum of GAMA and N-acetyl-S-(1-carbamoyl-2-hydroxyethyl)-L-cysteine (iso-GAMA). Thus, AAMA-sul may alternatively become a specific biomarker for investigating the acrylamide exposure in humans. Current proposed method provides a substantial methodology support for comprehensive

  4. 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

  5. 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

  6. Development, validation and application of an ultra high performance liquid chromatographic-tandem mass spectrometric method for the simultaneous detection and quantification of five different classes of veterinary antibiotics in swine manure.

    Science.gov (United States)

    Van den Meersche, Tina; Van Pamel, Els; Van Poucke, Christof; Herman, Lieve; Heyndrickx, Marc; Rasschaert, Geertrui; Daeseleire, Els

    2016-01-15

    In this study, a fast, simple and selective ultra high performance liquid chromatographic-tandem mass spectrometric (UHPLC-MS/MS) method for the simultaneous detection and quantification of colistin, sulfadiazine, trimethoprim, doxycycline, oxytetracycline and ceftiofur and for the detection of tylosin A in swine manure was developed and validated. First, a simple extraction procedure with acetonitrile and 6% trichloroacetic acid was carried out. Second, the supernatant was evaporated and the pellet was reconstituted in 1 ml of water/acetonitrile (80/20) and 0.1% formic acid. Extracts were filtered and analyzed by UHPLC-MS/MS on a Kinetex C18 column using gradient elution. The method developed was validated according to the criteria of Commission Decision 2002/657/EC. Recovery percentages varied between 94% and 106%, repeatability percentages were within the range of 1.7-9.2% and the intralaboratory reproducibility varied between 2.8% and 9.3% for all compounds, except for tylosin A for which more variation was observed resulting in a higher measurement uncertainty. The limit of detection and limit of quantification varied between 1.1 and 20.2 and between 3.5 and 67.3 μg/kg, respectively. This method was used to determine the presence and concentration of the seven antibiotic residues in swine manure sampled from ten different manure pits on farms where the selected antibiotics were used. A link was found between the antibiotics used and detected, except for ceftiofur which is injected at low doses and degraded readily in swine manure and was therefore not recovered in any of the samples. To the best of our knowledge, this is the first method available for the simultaneous extraction and quantification of colistin with other antibiotic classes. Additionally, colistin was never extracted from swine manure before. Another innovative aspect of this method is the simultaneous detection and quantification of five different classes of antibiotic residues in swine manure

  7. Identification of regioisomers of methylated kaempferol and quercetin by ultra high performance liquid chromatography quadrupole time-of-flight (UHPLC–QTOF) tandem mass spectrometry combined with diagnostic fragmentation pattern analysis

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Chengying; Lv, Haipeng; Zhang, Xinzhong; Chen, Zongmao; Shi, Jiang [Tea Research Institute, Chinese Academy of Agricultural Sciences, 9 Meiling South Road, Hangzhou, Zhejiang 310008 (China); Lu, Meiling, E-mail: meilinglu@hotmail.com [Chemical Analysis Group, Agilent Technologies, No. 3 Wangjing North Road, Chaoyang Distr., Beijing 100102 (China); Lin, Zhi, E-mail: linz@mail.tricaas.com [Tea Research Institute, Chinese Academy of Agricultural Sciences, 9 Meiling South Road, Hangzhou, Zhejiang 310008 (China)

    2013-09-17

    Highlights: •Found methane elimination is position-specific for methylated flavonols. •Found retro Diels–Alder fragments retained methoxy at original ring of flavonols. •Proposed a diagnostic pattern for discriminating regioisomers of flavonols. •Identified the specificity of three novel flavonol O-methyltransferases. •Identified six biologically active compounds and four new compounds. -- Abstract: The O-methylation of active flavonoids can enhance their antiallergic, anticancerous, and cardioprotective effects depending on the methylation position. Thus, it is biologically and pharmacologically important to differentiate methylated flavonoid regioisomers. In this study, we examined the regioisomers of methylated kaempferol and quercetin using ultra high performance liquid chromatography quadrupole time-of-flight tandem mass spectrometry. The methyl groups on the flavonoids can generally be cleaved as methyl radicals in a position-independent manner. We found that methyl groups can be cleaved as methane. If there are protons adjacent the methoxy on the flavonol rings, intra-molecule proton transfer can occur via collision-induced dissociation, and one molecule of methane can then be eliminated. The remaining charged fragment ([M+H−CH{sub 4}]{sup +}) reflects the adjacent structure and is specific to the methoxy position. Furthermore, the retro Diels–Alder (RDA) fragmentation of methylated flavonols can generate fragments with the methoxy at the original methylated ring. Combining the position-specific [M+H−CH{sub 4}]{sup +} fragment with the RDA fragments provides a diagnostic pattern for rapidly identifying methylated regioisomeric flavonols. Along with their retention behaviour, we have successfully identified ten regioisomers of methylated kaempferol and quercetin, which include six compounds previously reported in plants and shown to be biologically active. The developed approach is sensitive, rapid, reliable, and requires few standard

  8. Simultaneous Determination of Purpurin, Munjistin and Mollugin in Rat Plasma by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry: Application to a Pharmacokinetic Study after Oral Administration of Rubia cordifolia L. Extract

    Directory of Open Access Journals (Sweden)

    Mingjie Gao

    2016-06-01

    Full Text Available A specific, simple, sensitive Ultra High Performance Liquid Chromatography-tandem Mass Spectrometry (UHPLC-MS/MS method has been developed and validated for the simultaneous determination and pharmacokinetic study of purpurin, munjistin, and mollugin in rat plasma. Chromatographic separation was carried out using a C18 column (ACQUITY UPLC® HSS T3, 1.8 μm, 2.1 × 100 mm with gradient elution. The compounds were detected on a 6430 triple-quadrupole tandem MS with an electrospray ionization (ESI interface using multiple reaction monitoring (MRM in positive ionization mode. The samples were prepared by a liquid-liquid extraction (LLE method with ethyl acetate after being spiked with an internal standard (bifendate. The current UHPLC-MS/MS assay was validated for its linearity, intra-day and inter-day precisions, accuracy, extraction recovery, matrix effect and stability in different conditions. The method was linear for all analytes over the investigated range with all determined correlation coefficients exceeding 0.9900. The intra-day and inter-day precisions were in the range of 4.21% to 14.84%, and the relative errors of accuracies were in the range of −14.05% to 14.75%. The mean recoveries and matrix effects of purpurin, munjistin, and mollugin were higher than 78.87% and 92.56%, repectively. After oral administration of 0.82 g/kg of Rubia cordifolia extract, the maximum plasma concentrations (Cmax were 70.10 ± 11.78 ng/mL for purpurin, 26.09 ± 6.6 ng/mL for munjistin, and 52.10 ± 6.71 ng/mL for mollugin. The time for maximal concentration (Tmax was 1.61 ± 0.24 h for purpurin, 2.58 ± 0.19 h for munjistin, and 1.99 ± 0.21 h for mollugin. The established method was further applied to a pharmacokinetic study of purpurin, munjistin, and mollugin in rat plasma. It was concluded from the pharmacokinetic parameters that the three analytes showed a process of slow absorption and metabolism after oral administration of R. cordifolia extract to

  9. RESOLVE AND ECO: THE HALO MASS-DEPENDENT SHAPE OF GALAXY STELLAR AND BARYONIC MASS FUNCTIONS

    Energy Technology Data Exchange (ETDEWEB)

    Eckert, Kathleen D.; Kannappan, Sheila J.; Stark, David V.; Moffett, Amanda J.; Norris, Mark A. [Department of Physics and Astronomy, University of North Carolina, 141 Chapman Hall CB 3255, Chapel Hill, NC 27599 (United States); Berlind, Andreas A., E-mail: keckert@physics.unc.edu [International Centre for Radio Astronomy Research (ICRAR), The University of Western Australia, 35 Stirling Highway, Crawley, WA 6009 (Australia)

    2016-06-20

    In this work, we present galaxy stellar and baryonic (stars plus cold gas) mass functions (SMF and BMF) and their halo mass dependence for two volume-limited data sets. The first, RESOLVE-B, coincides with the Stripe 82 footprint and is extremely complete down to baryonic mass M {sub bary} ∼ 10{sup 9.1} M {sub ⊙}, probing the gas-rich dwarf regime below M {sub bary} ∼ 10{sup 10} M {sub ⊙}. The second, ECO, covers a ∼40× larger volume (containing RESOLVE-A) and is complete to M {sub bary} ∼ 10{sup 9.4} M {sub ⊙}. To construct the SMF and BMF we implement a new “cross-bin sampling” technique with Monte Carlo sampling from the full likelihood distributions of stellar or baryonic mass. Our SMFs exhibit the “plateau” feature starting below M {sub star} ∼ 10{sup 10} M {sub ⊙} that has been described in prior work. However, the BMF fills in this feature and rises as a straight power law below ∼10{sup 10} M {sub ⊙}, as gas-dominated galaxies become the majority of the population. Nonetheless, the low-mass slope of the BMF is not as steep as that of the theoretical dark matter halo MF. Moreover, we assign group halo masses by abundance matching, finding that the SMF and BMF, separated into four physically motivated halo mass regimes, reveal complex structure underlying the simple shape of the overall MFs. In particular, the satellite MFs are depressed below the central galaxy MF “humps” in groups with mass <10{sup 13.5} M {sub ⊙} yet rise steeply in clusters. Our results suggest that satellite destruction and stripping are active from the point of nascent group formation. We show that the key role of groups in shaping MFs enables reconstruction of a given survey’s SMF or BMF based on its group halo mass distribution.

  10. An Ultra-Sensitive, Size Resolved Particle Mass Measurement Device, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — By providing size resolved compositional information, the Aerosol Mass Spectrometer (AMS) has greatly advanced understanding of aircraft particulate matter (PM)...

  11. An Ultra-Sensitive, Size Resolved Particle Mass Measurement Device, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — The characterization of aircraft particulate matter (PM) emissions has benefited greatly by the Aerosol Mass Spectrometer (AMS) by providing size resolved...

  12. Ultra high-energy cosmic ray composition

    International Nuclear Information System (INIS)

    Longley, N.P.

    1993-01-01

    The Soudan 2 surface-underground cosmic ray experiment can simultaneously measure surface shower size, underground muon multiplicity, and underground muon separation for ultra high energy cosmic ray showers. These measurements are sensitive to the primary composition. Analysis for energies from 10 1 to 10 4 TeV favors a light flux consisting of predominantly H and He nuclei

  13. Sintering of ultra high molecular weight polyethylene

    Indian Academy of Sciences (India)

    Abstract. Ultra high molecular weight polyethylene (UHMWPE) is a high performance polymer having low coefficient of friction, good abrasion resistance, good chemical ... In this study, we report our results on compaction and sintering behaviour of two grades of UHMWPE with reference to the powder morphology, sintering ...

  14. Expectations for ultra-high energy interactions

    International Nuclear Information System (INIS)

    Feynman, R.P.

    1978-01-01

    Strong interactions at ultra-high energies are discussed with emphasis on the hadrons produced in high energy collisions. Evidence is considered that quantum chromodynamics might be the right theory, and also some estimates are given of quantum chromodynamics asymptotic-freedom phenomena, the work under discussion being very preliminary. 6 references

  15. Scaling violations at ultra-high energies

    International Nuclear Information System (INIS)

    Tung, W.K.

    1979-01-01

    The paper discusses some of the features of high energy lepton-hadron scattering, including the observed (Bjorken) scaling behavior. The cross-sections where all hadron final states are summed over, are examined and the general formulas for the differential cross-section are examined. The subjects of scaling, breaking and phenomenological consequences are studied, and a list of what ultra-high energy neutrino physics can teach QCD is given

  16. Charge and frequency resolved isochronous mass spectrometry and the mass of 51Co

    International Nuclear Information System (INIS)

    Shuai, P.; Xu, H.S.; Tu, X.L.; Zhang, Y.H.; Sun, B.H.; Wang, M.

    2014-01-01

    Revolution frequency measurements of individual ions in storage rings require sophisticated timing detectors. One of common approaches for such detectors is the detection of secondary electrons released from a thin foil due to penetration of the stored ions. A new method based on the analysis of intensities of secondary electrons was developed which enables determination of the charge of each ion simultaneously with the measurement of its revolution frequency. Although the mass-over-charge ratios of 51 Co 27+ and 34 Ar 18+ ions are almost identical, and therefore, the ions cannot be resolved in a storage ring, by applying the new method the mass excess of the short-lived 51 Co is determined for the first time to be ME( 51 Co)=−27342(48) keV. Shell-model calculations in the fp-shell nuclei compared to the new data indicate the need to include isospin-nonconserving forces

  17. Ultra high field magnetic resonance imaging

    International Nuclear Information System (INIS)

    Lethimonnier, F.; Vedrine, P.

    2007-01-01

    Understanding human brain function, brain development and brain dysfunction is one of the great challenges of the twenty first century. Biomedical imaging has now run up against a number of technical constraints that are exposing limits to its potential. In order to overcome the current limits to high-field magnetic resonance cerebral imaging (MRI) and unleash its fullest potential, the Cea has built NeuroSpin, an ultra-high-field neuroimaging facility at its Saclay centre (in the Essonne). NeuroSpin already boasts three fully operational MRI systems. The first is a 3-tesla high-field system and the second is a very-high-field 7-tesla system, both of which are dedicated to clinical studies and investigations in humans, while the third is an ultra-high-field 17.65-tesla system designed for studies on small animals. In 2011, NeuroSpin will be commissioning an 11.7-tesla ultra-high-field system of unprecedented power that is designed for research on human subjects. The level of the magnetic field and the scale required will make this joint French-German project to build the magnet a breakthrough in the international arena. (authors)

  18. Low velocity impact behaviour of ultra high strength concrete panels

    Indian Academy of Sciences (India)

    Ultra high strength concrete; panel; drop weight test; impact analysis;. ABAQUS. 1. Introduction. Ultra high strength concrete ... Knight (2012) investigated the dynamic behaviour of steel fibre reinforced concrete plates under impact loading with ...

  19. Ultra-high vacuum technology for accelerators

    CERN Multimedia

    CERN. Geneva. Audiovisual Unit; Hilleret, Noël; Strubin, Pierre M

    2002-01-01

    The lectures will start with a review of the basics of vacuum physics required to build Ultra High Vacuum (UHV) systems, such as static and dynamic outgassing. Before reviewing the various pumping and measurement devices, including the most modern one like Non Evaporable Getter (NEG) coatings, an overview of adequate materials to be used in UHV systems will be given together with their treatment (e.g. cleaning procedures and bake out). Practical examples based on existing or future accelerators will be used to illustrate the topics. Finally, a short overview of modern vacuum controls and interlocks will be given.

  20. Ultra-high vacuum photoelectron linear accelerator

    Science.gov (United States)

    Yu, David U.L.; Luo, Yan

    2013-07-16

    An rf linear accelerator for producing an electron beam. The outer wall of the rf cavity of said linear accelerator being perforated to allow gas inside said rf cavity to flow to a pressure chamber surrounding said rf cavity and having means of ultra high vacuum pumping of the cathode of said rf linear accelerator. Said rf linear accelerator is used to accelerate polarized or unpolarized electrons produced by a photocathode, or to accelerate thermally heated electrons produced by a thermionic cathode, or to accelerate rf heated field emission electrons produced by a field emission cathode.

  1. Ultra-high resolution protein crystallography

    International Nuclear Information System (INIS)

    Takeda, Kazuki; Hirano, Yu; Miki, Kunio

    2010-01-01

    Many protein structures have been determined by X-ray crystallography and deposited with the Protein Data Bank. However, these structures at usual resolution (1.5< d<3.0 A) are insufficient in their precision and quantity for elucidating the molecular mechanism of protein functions directly from structural information. Several studies at ultra-high resolution (d<0.8 A) have been performed with synchrotron radiation in the last decade. The highest resolution of the protein crystals was achieved at 0.54 A resolution for a small protein, crambin. In such high resolution crystals, almost all of hydrogen atoms of proteins and some hydrogen atoms of bound water molecules are experimentally observed. In addition, outer-shell electrons of proteins can be analyzed by the multipole refinement procedure. However, the influence of X-rays should be precisely estimated in order to derive meaningful information from the crystallographic results. In this review, we summarize refinement procedures, current status and perspectives for ultra high resolution protein crystallography. (author)

  2. A simple multi-residue method for the determination of pesticides in fruits and vegetables using a methanolic extraction and ultra-high-performance liquid chromatography-tandem mass spectrometry: optimization and extension of scope.

    Science.gov (United States)

    Hanot, V; Goscinny, S; Deridder, M

    2015-03-06

    In 2004, a new multi-residue pesticides method had been published using methanol as extraction solvent. Our goal for this study was to optimize the analytical scheme while extending the compound scope from 19 to 200 pesticides. The main changes from the original method take place at the sample extraction and processing with a special attention to make the overall method fit for routine analysis with minimal cost. Hence, after a quick Ultra-Turrax homogenization with a methanolic solution, the sample is simply diluted before the separation and detection by ultra-high-performance liquid chromatography and MS/MS detection for quantitative and confirmatory purposes. The performance of the method including limits of quantification (LOQs), linearity, matrix effect, precision was evaluated during validation in accordance with the European Union SANCO/12571/2013 regulatory guidelines. Two representative matrices, lettuce and orange, were selected and fortified at two concentration levels for these experiments. At the LOQ and ten times the LOQ, recoveries of the analytes were mostly within 70-120%, with coefficients of variation lower than 25% in intra-day repeatability conditions. In addition to being simple and fast, these results demonstrate the suitability of the optimized method for the analysis of large scope pesticides in routine laboratories. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Analysis of eleven phenolic compounds including novel p-coumaroyl derivatives in lettuce (Lactuca sativa L.) by ultra-high-performance liquid chromatography with photodiode array and mass spectrometry detection.

    Science.gov (United States)

    Ribas-Agustí, Albert; Gratacós-Cubarsí, Marta; Sárraga, Carmen; García-Regueiro, José-Antonio; Castellari, Massimo

    2011-01-01

    Lettuce is a widely consumed vegetable and a good source of phenolic compounds. Several factors (genetic, agronomical and environmental) can influence the lettuce composition; their effects are not completely defined and more studies are needed on this topic. To develop an improved ultra-high-performance liquid chromatography (UHPLC) method to quantify the main target intact phenolic compounds in lettuce. UHPLC identification of the compounds was supported by PAD spectra and MS(n) analyses. Quantification was carried out by PAD, by creating matrix-matched calibration curves at the specific wavelength for each compound. Sample pretreatment was simplified, with neither purification nor hydrolysis steps. Chromatographic conditions were chosen to minimise matrix interferences and to give a suitable separation of the major phenolic compounds within 27 min. The method allowed the quantification of 11 intact phenolic compounds in Romaine lettuces, including phenolic acids (caffeoyl and p-coumaroyl esters) and flavonoids (quercetin glycosides). Four p-coumaroyl esters were tentatively identified and quantified for the first time in lettuce. The main intact phenolic compounds, including four novel p-coumaroyl esters, were simultaneously quantified in lettuce with optimal performances and a reduced total time of analysis. These findings make headway in the understanding of the lettuce phytochemicals with potential nutritional relevance. Copyright © 2011 John Wiley & Sons, Ltd.

  4. Development of a sensitive determination method for benzotriazole UV stabilizers in enviromental water samples with stir bar sorption extraction and liquid desorption prior to ultra-high performance liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Montesdeoca-Esponda, Sarah; del Toro-Moreno, Adrián; Sosa-Ferrera, Zoraida; Santana-Rodríguez, José Juan

    2013-07-01

    Benzotriazole UV stabilizers are emerging compounds used in personal care products and can enter surface water after passing through wastewater treatment plants without being removed. Because these analytes are strongly hydrophobic, there is an environmental risk of accumulation in solid matrices and magnification through the trophic chain. In this work, a method based on stir bar sorption extraction with liquid desorption is presented for the extraction of benzotriazole UV stabilizers from water samples. Stir bar sorptive extraction was combined with ultra-high performance LC with MS/MS detection. All important factors affecting the stir bar sorptive extraction procedure are discussed, and the optimized method was applied to seawater and wastewater samples from Gran Canaria Island, providing good selectivity and sensitivity with LODs and limits of quantification in the range of 18.4-55.1 and 61.5-184 ng/L, respectively. Recoveries between 68.4-92.2% were achieved for the more polar compounds, whereas the recoveries were lower for the two less polar compounds, most likely due to their strong absorption into the polydimethylsiloxane stir bar phase that does not allows the complete desorption. The repeatability studies gave RSDs of between 6.45 and 12.6% for all compounds in the real samples. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Test Sample for the Spatially Resolved Quantification of Illicit Drugs on Fingerprints Using Imaging Mass Spectrometry

    NARCIS (Netherlands)

    Muramoto, S.; Forbes, T.P.; van Asten, A.C.; Gillen, G.

    2015-01-01

    A novel test sample for the spatially resolved quantification of illicit drugs on the surface of a fingerprint using time-of-flight secondary ion mass spectrometry (ToF-SIMS) and desorption electrospray ionization mass spectrometry (DESI-MS) was demonstrated. Calibration curves relating the signal

  6. Detecting ultra high energy neutrinos with LOFAR

    International Nuclear Information System (INIS)

    Mevius, M.; Buitink, S.; Falcke, H.; Hörandel, J.; James, C.W.; McFadden, R.; Scholten, O.; Singh, K.; Stappers, B.; Veen, S. ter

    2012-01-01

    The NuMoon project aims to detect signals of Ultra High Energy (UHE) Cosmic Rays with radio telescopes on Earth using the Lunar Cherenkov technique at low frequencies (∼150MHz). The advantage of using low frequencies is the much larger effective detecting volume, with as trade-off the cut-off in sensitivity at lower energies. A first upper limit on the UHE neutrino flux from data of the Westerbork Radio Telescope (WSRT) has been published, while a second experiment, using the new LOFAR telescope, is in preparation. The advantages of LOFAR over WSRT are the larger collecting area, the better pointing accuracy and the use of ring buffers, which allow the implementation of a sophisticated self-trigger algorithm. The expected sensitivity of LOFAR reaches flux limits within the range of some theoretical production models.

  7. Multilayer ultra-high-temperature ceramic coatings

    Science.gov (United States)

    Loehman, Ronald E [Albuquerque, NM; Corral, Erica L [Tucson, AZ

    2012-03-20

    A coated carbon-carbon composite material with multiple ceramic layers to provide oxidation protection from ultra-high-temperatures, where if the carbon-carbon composite material is uninhibited with B.sub.4C particles, then the first layer on the composite material is selected from ZrB.sub.2 and HfB.sub.2, onto which is coated a layer of SiC coated and if the carbon-carbon composite material is inhibited with B.sub.4C particles, then protection can be achieved with a layer of SiC and a layer of either ZrB.sub.2 and HfB.sub.2 in any order.

  8. Ultra-High-Energy Cosmic Rays

    CERN Document Server

    Dova, M.T.

    2015-05-22

    The origin of the ultra high energy cosmic rays (UHECR) with energies above E > 10 17 eV, is still unknown. The discovery of their sources will reveal the engines of the most energetic astrophysical accelerators in the universe. This is a written version of a series of lectures devoted to UHECR at the 2013 CERN-Latin-American School of High-Energy Physics. We present anintroduction to acceleration mechanisms of charged particles to the highest energies in astrophysical objects, their propagation from the sources to Earth, and the experimental techniques for their detection. We also discuss some of the relevant observational results from Telescope Array and Pierre Auger Observatory. These experiments deal with particle interactions at energies orders of magnitude higher than achieved in terrestrial accelerators.

  9. Active Galactic Nuclei: Sources for ultra high energy cosmic rays?

    International Nuclear Information System (INIS)

    Biermann, Peter L.; Becker, Julia K.; Caramete, Laurentiu; Curutiu, Alex; Engel, Ralph; Falcke, Heino; Gergely, Laszlo A.; Isar, P. Gina; Maris, Ioana C.; Meli, Athina; Kampert, Karl-Heinz; Stanev, Todor; Tascau, Oana; Zier, Christian

    2009-01-01

    The origin of ultra high energy cosmic rays promises to lead us to a deeper understanding of the structure of matter. This is possible through the study of particle collisions at center-of-mass energies in interactions far larger than anything possible with the Large Hadron Collider, albeit at the substantial cost of no control over the sources and interaction sites. For the extreme energies we have to identify and understand the sources first, before trying to use them as physics laboratories. Here we describe the current stage of this exploration. The most promising contenders as sources are radio galaxies and gamma ray bursts. The sky distribution of observed events yields a hint favoring radio galaxies. Key in this quest are the intergalactic and galactic magnetic fields, whose strength and structure are not yet fully understood. Current data and statistics do not yet allow a final judgement. We outline how we may progress in the near future.

  10. Active Galactic Nuclei: Sources for ultra high energy cosmic rays?

    Energy Technology Data Exchange (ETDEWEB)

    Biermann, Peter L. [MPI for Radioastronomy, Bonn (Germany); Dept. of Phys. and Astron., Univ. of Bonn (Germany); Dept. of Phys. and Astr., Univ. of Alabama, Tuscaloosa, AL (United States); Dept. of Phys., Univ. of Alabama at Huntsville, AL (United States); Inst. Nucl. Phys. FZ, Karlsruhe Inst. of Techn. (KIT) (Germany); Becker, Julia K. [Institution foer Fysik, Goeteborgs Univ. (Sweden); Dept. of Phys., Univ. Dortmund, Dortmund (Germany); Caramete, Laurentiu [MPI for Radioastronomy, Bonn (Germany); Institute for Space Studies, Bucharest (Romania); Curutiu, Alex [MPI for Radioastronomy, Bonn (Germany); Engel, Ralph [Inst. Nucl. Phys. FZ, Karlsruhe Inst. of Techn. (KIT) (Germany); Falcke, Heino [Dept. of Astrophys., IMAP, Radboud Univ., Nijmegen (Netherlands); ASTRON, Dwingeloo (Netherlands); Gergely, Laszlo A. [Dept. Appl. Sci., London South Bank University (United Kingdom); Dept. of Theoret. and Exp. Phys., Univ. of Szeged, Szeged (Hungary); Isar, P. Gina [Inst. Nucl. Phys. FZ, Karlsruhe Inst. of Techn. (KIT) (Germany); Institute for Space Studies, Bucharest (Romania); Maris, Ioana C. [Inst. Nucl. Phys. FZ, Karlsruhe Inst. of Techn. (KIT) (Germany); Meli, Athina [Physik. Inst. Univ. Erlangen-Nuernberg (Germany); Kampert, Karl-Heinz [Phys. Dept., Univ. Wuppertal (Germany); Stanev, Todor [Bartol Research Inst., Univ. of Delaware, Newark, DE (United States); Tascau, Oana [Phys. Dept., Univ. Wuppertal (Germany); Zier, Christian [MPI for Radioastronomy, Bonn (Germany); Raman Res. Inst., Bangalore (India)

    2009-05-15

    The origin of ultra high energy cosmic rays promises to lead us to a deeper understanding of the structure of matter. This is possible through the study of particle collisions at center-of-mass energies in interactions far larger than anything possible with the Large Hadron Collider, albeit at the substantial cost of no control over the sources and interaction sites. For the extreme energies we have to identify and understand the sources first, before trying to use them as physics laboratories. Here we describe the current stage of this exploration. The most promising contenders as sources are radio galaxies and gamma ray bursts. The sky distribution of observed events yields a hint favoring radio galaxies. Key in this quest are the intergalactic and galactic magnetic fields, whose strength and structure are not yet fully understood. Current data and statistics do not yet allow a final judgement. We outline how we may progress in the near future.

  11. Ultra high energy cosmic rays above 10 GeV: Hints to new physics ...

    Indian Academy of Sciences (India)

    Ultra high energy cosmic rays; physics beyond standard model. ... The origin of the observed cosmic ray (CR) events above 10ѕј eV — the so-called ex- .... to arise simply from decay of some supermassive particles (of mass> 10ѕЅ eV) ...

  12. REMOVING BIASES IN RESOLVED STELLAR MASS MAPS OF GALAXY DISKS THROUGH SUCCESSIVE BAYESIAN MARGINALIZATION

    Energy Technology Data Exchange (ETDEWEB)

    Martínez-García, Eric E. [Cerrada del Rey 40-A, Chimalcoyoc Tlalpan, Ciudad de México, C.P. 14630, México (Mexico); González-Lópezlira, Rosa A.; Bruzual A, Gustavo [Instituto de Radioastronomía y Astrofísica, UNAM, Campus Morelia, Michoacán, C.P. 58089, México (Mexico); Magris C, Gladis, E-mail: martinezgarciaeric@gmail.com [Centro de Investigaciones de Astronomía, Apartado Postal 264, Mérida 5101-A (Venezuela, Bolivarian Republic of)

    2017-01-20

    Stellar masses of galaxies are frequently obtained by fitting stellar population synthesis models to galaxy photometry or spectra. The state of the art method resolves spatial structures within a galaxy to assess the total stellar mass content. In comparison to unresolved studies, resolved methods yield, on average, higher fractions of stellar mass for galaxies. In this work we improve the current method in order to mitigate a bias related to the resolved spatial distribution derived for the mass. The bias consists in an apparent filamentary mass distribution and a spatial coincidence between mass structures and dust lanes near spiral arms. The improved method is based on iterative Bayesian marginalization, through a new algorithm we have named Bayesian Successive Priors (BSP). We have applied BSP to M51 and to a pilot sample of 90 spiral galaxies from the Ohio State University Bright Spiral Galaxy Survey. By quantitatively comparing both methods, we find that the average fraction of stellar mass missed by unresolved studies is only half what previously thought. In contrast with the previous method, the output BSP mass maps bear a better resemblance to near-infrared images.

  13. Ultra high performance concrete dematerialization study

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2004-03-01

    Concrete is the most widely used building material in the world and its use is expected to grow. It is well recognized that the production of portland cement results in the release of large amounts of carbon dioxide, a greenhouse gas (GHG). The main challenge facing the industry is to produce concrete in an environmentally sustainable manner. Reclaimed industrial by-proudcts such as fly ash, silica fume and slag can reduce the amount of portland cement needed to make concrete, thereby reducing the amount of GHGs released to the atmosphere. The use of these supplementary cementing materials (SCM) can also enhance the long-term strength and durability of concrete. The intention of the EcoSmart{sup TM} Concrete Project is to develop sustainable concrete through innovation in supply, design and construction. In particular, the project focuses on finding a way to minimize the GHG signature of concrete by maximizing the replacement of portland cement in the concrete mix with SCM while improving the cost, performance and constructability. This paper describes the use of Ductal{sup R} Ultra High Performance Concrete (UHPC) for ramps in a condominium. It examined the relationship between the selection of UHPC and the overall environmental performance, cost, constructability maintenance and operational efficiency as it relates to the EcoSmart Program. The advantages and challenges of using UHPC were outlined. In addition to its very high strength, UHPC has been shown to have very good potential for GHG emission reduction due to the reduced material requirements, reduced transport costs and increased SCM content. refs., tabs., figs.

  14. Preferential alkali metal adduct formation by cis geometrical isomers of dicaffeoylquinic acids allows for efficient discrimination from their trans isomers during ultra-high-performance liquid chromatography/quadrupole time-of-flight mass spectrometry

    CSIR Research Space (South Africa)

    Makola, MM

    2016-03-01

    Full Text Available distinguish between various isomers of flavonoid glycosides, but were able to obtain structural information such as the site of glycosylation on the flavonoid. The metal binding of catechol-containing molecules has also been known for a long time... with serious biological and chemical implications.[34] In mass spectrometry studies, the metal binding/chelation by catechol-containing flavonoids has been noted and used to discriminate between closely related molecules.[35] In the current study...

  15. An ultra high performance liquid chromatography with tandem mass spectrometry method for plasma and cerebrospinal fluid pharmacokinetics of rhein in patients with traumatic brain injury after administration of rhubarb decoction.

    Science.gov (United States)

    Wang, Yang; Fan, Rong; Luo, Jiekun; Tang, Tao; Xing, Zhihua; Xia, Zian; Peng, Weijun; Wang, Wenzhu; Lv, Huiying; Huang, Wei; Liang, Yizeng; Yi, Lunzhao; Lu, Hongmei; Huang, Xi

    2015-04-01

    Damage of blood-brain barrier is a common result of traumatic brain injury. This damage can open the blood-brain barrier and allow drug passage. An ultraperformance liquid chromatography with tandem mass spectrometry method was established to determine the concentration of rhein in the biofluids (plasma and cerebrospinal fluid) of patients with a compromised blood-brain barrier following traumatic brain injury after rhubarb administration. Furthermore, the pharmacokinetic profiles were analyzed. A triple-quadruple tandem mass spectrometer with electrospray ionization was used for rhein detection. The mass transition followed was m/z 283.06→239.0. The calibration curve was linear in the concentration range of 10-8000 ng/mL for the biofluids. The intra- and interday precisions were less than 10%. The relative standard deviation of recovery was less than 15% in biological matrices. The pharmacokinetic data showed that rhein was rapidly transported into biofluids, and exhibited a peak concentration 1 h after rhubarb administration. The elimination rate of rhein was slow. The AUCcerebrospinal fluid /AUCplasma (AUC is area under curve) of rhein was approximately 17%, indicating that portions of rhein could pass the impaired blood-brain barrier. The method was successfully applied to quantify rhein in the biofluids of all patients. The data presented can help to guide clinical applications of rhubarb for treating traumatic brain injury. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Antarctic Mass Loss from GRACE from Space- and Time-Resolved Modeling with Slepian Functions

    Science.gov (United States)

    Simons, F. J.; Harig, C.

    2013-12-01

    The melting of polar ice sheets is a major contributor to global sea-level rise. Antarctica is of particular interest since most of the mass loss has occurred in West Antarctica, however updated glacial isostatic adjustment (GIA) models and recent mass gains in East Antarctica have reduced the continent-wide integrated decadal trend of mass loss. Here we present a spatially and temporally resolved estimation of the Antarctic ice mass change using Slepian localization functions. With a Slepian basis specifically for Antarctica, the basis functions maximize their energy on the continent and we can project the geopotential fields into a sparse set of orthogonal coefficients. By fitting polynomial functions to the limited basis coefficients we maximize signal-to-noise levels and need not perform smoothing or destriping filters common to other approaches. In addition we determine an empirical noise covariance matrix from the GRACE data to estimate the uncertainty of mass estimation. When applied to large ice sheets, as in our own recent Greenland work, this technique is able to resolve both the overall continental integrated mass trend, as well as the spatial distribution of the mass changes over time. Using CSR-RL05 GRACE data between Jan. 2003 and Jan 2013, we estimate the regional accelerations in mass change for several sub-regions and examine how the spatial pattern of mass has changed. The Amundsen Sea coast of West Antarctica has experienced a large acceleration in mass loss (-26 Gt/yr^2). While mass loss is concentrated near Pine Island and Thwaites glaciers, it has also increased along the coast further towards the Ross ice shelf.

  17. Mass resolved angular distribution of fission products in 20Ne + 232Th reaction

    International Nuclear Information System (INIS)

    Tripathi, R.; Sodaye, S.; Sudarshan, K.; Kumar, Amit; Guin, R.

    2011-01-01

    Mass resolved angular distribution of fission products was measured in 20 Ne + 232 Th reaction at beam energy of 120 MeV. A preliminary analysis of the angular distribution data of fission products shows higher average anisotropy compared to that calculated using statistical theory. A signature of rise in anisotropy near symmetry, as reported in earlier studies in literature, is also seen. Further study is in progress to get more detailed information about the contribution from non-compound nucleus fission and dependence of angular anisotropy on asymmetry of mass division

  18. Optimization and application of parallel solid-phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry for the determination of 11 aminoglycoside residues in honey and royal jelly.

    Science.gov (United States)

    Wang, Xinran; Yang, Shupeng; Li, Yi; Zhang, Jinzhen; Jin, Yue; Zhao, Wen; Zhang, Yongxin; Huang, Jingping; Wang, Peng; Wu, Cuiling; Zhou, Jinhui

    2018-03-23

    A robust and sensitive method of solid-phase extraction followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was established and performed for the simultaneous determination of eleven aminoglycosides (AGs) in royal jelly and honey. After sample extraction by a phosphate buffer containing trichloroacetic acid (TCA) and ethylenediaminetetracetic acid disodium salt (Na 2 EDTA), the extraction solution was subjected to a parallel solid-phase extraction for clean-up prior to the LC-MS/MS analysis. The same method was applied to analyze two completely different matrices, honey and royal jelly. Good sensitivity, repeatability, and recovery were obtained by using the mobile phase without an ion-pairing reagent such as heptafluorobutyric acid (HFBA) or sodium heptanesulfonate. The calibration curves of the honey and royal jelly samples exhibited a good linear response (R 2  > 0.99) at six concentrations in the range of 10-1000 μg/mL. The limit of quantification (LOQ) of the AGs ranged from 10 to 25 μg/kg in the honey and from 12.5 to 25 μg/kg in the royal jelly. The recoveries of the AGs for the honey and royal jelly samples were in the range of 79.48% to 108.95% and 74.61% to 113.70% respectively and the relative standard deviations (RSDs) were between 1.23% and 9.59%, and between 1.51% and 9.98%, respectively. The proposed approach has been allowed in China as a reference method for the simultaneous determination of eleven AGs in honey and royal jelly. Copyright © 2018 Elsevier B.V. All rights reserved.

  19. Ultra(high)-pressure liquid chromatography-electrospray ionization-time-of-flight-ion mobility-high definition mass spectrometry for the rapid identification and structural characterization of flavonoid glycosides from cauliflower waste.

    Science.gov (United States)

    Gonzales, Gerard Bryan; Raes, Katleen; Coelus, Sofie; Struijs, Karin; Smagghe, Guy; Van Camp, John

    2014-01-03

    In this paper, a strategy for the detection and structural elucidation of flavonoid glycosides from a complex matrix in a single chromatographic run using U(H)PLC-ESI-IMS-HDMS/MS(E) is presented. This system operates using alternative low and high energy voltages that is able to perform the task of conventional MS/MS in a data-independent way without re-injection of the sample, which saves analytical time. Also, ion mobility separation (IMS) was employed as an additional separation technique for compounds that are co-eluting after U(H)PLC separation. First, the fragmentation of flavonoid standards were analyzed and criteria was set for structural elucidation of flavonoids in a plant extract. Based on retention times, UV spectra, exact mass, and MS fragment characteristics, such as abundances of daughter ions and the presence of radical ions ([Y0-H](-)), a total 19 flavonoid glycosides, of which 8 non-acylated and 11 acylated, were detected and structurally characterized in a cauliflower waste extract. Kaempferol and quercetin were the main aglycones detected while sinapic and ferulic acid were the main phenolic acids. C-glycosides were also found although their structure could not be elucidated. The proposed method can be used as a rapid screening test for flavonoid identification and for routine analysis of plant extracts, such as these derived from cauliflower waste. The study also confirms that agroindustrial wastes, such as cauliflower leaves, could be seen as a valuable source of different bioactive phenolic compounds. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Multiresidue analysis of oestrogenic compounds in cow, goat, sheep and human milk using core-shell polydopamine coated magnetic nanoparticles as extraction sorbent in micro-dispersive solid-phase extraction followed by ultra-high-performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Socas-Rodríguez, Bárbara; Hernández-Borges, Javier; Herrera-Herrera, Antonio V; Rodríguez-Delgado, Miguel Ángel

    2018-03-01

    In this work, the suitability of Fe 3 O 4 nanoparticles coated with polydopamine was evaluated as sorbent for the extraction of a group of 21 compounds with oestrogenic activity including seven phytoestrogens, six mycotoxins as well as four synthetic and four natural oestrogens from different types of milk, including sheep milk, in which the evaluation of oestrogenic compounds have never been developed before. Extraction was carried out using magnetic micro-dispersive solid-phase extraction after a previous deproteinisation step. Separation, determination and quantification of the target analytes were achieved by ultra-high-performance liquid chromatography coupled to triple quadrupole-tandem mass spectrometry. The methodology was validated for five milk samples using 17β-estradiol-2,4,16,16,17-d 5 as internal standard for natural and synthetic oestrogens, β-zearalanol-10,10,11,12,12-d 5 for mycotoxins and prunetin for phytoestrogens. Recovery values ranged from 70 to 120% for the five types of matrices with relative standard deviation values lower than 18%. Limits of quantification of the method were in the range 0.55-11.8 μg L -1 for all samples. Graphical abstract General scheme of the multiresidue analysis of oestrogenic compounds in milk using core-shell polydopamine coated magnetic nanoparticles as extraction sorbent in μ-dSPE.

  1. The profiling of the metabolites of hirsutine in rat by ultra-high performance liquid chromatography coupled with linear ion trap Orbitrap mass spectrometry: An improved strategy for the systematic screening and identification of metabolites in multi-samples in vivo.

    Science.gov (United States)

    Wang, Jianwei; Qi, Peng; Hou, Jinjun; Shen, Yao; Yang, Min; Bi, Qirui; Deng, Yanping; Shi, Xiaojian; Feng, Ruihong; Feng, Zijin; Wu, Wanying; Guo, Dean

    2017-02-05

    Drug metabolites identification and construction of metabolic profile are meaningful work for the drug discovery and development. The great challenge during this process is the work of the structural clarification of possible metabolites in the complicated biological matrix, which often resulting in a huge amount data sets, especially in multi-samples in vivo. Analyzing these complex data manually is time-consuming and laborious. The object of this study was to develop a practical strategy for screening and identifying of metabolites from multiple biological samples efficiently. Using hirsutine (HTI), an active components of Uncaria rhynchophylla (Gouteng in Chinese) as a model and its plasma, urine, bile, feces and various tissues were analyzed with data processing software (Metwork), data mining tool (Progenesis QI), and HR-MS n data by ultra-high performance liquid chromatography/linear ion trap-Orbitrap mass spectrometry (U-HPLC/LTQ-Orbitrap-MS). A total of 67 metabolites of HTI in rat biological samples were tentatively identified with established library, and to our knowledge most of which were reported for the first time. The possible metabolic pathways were subsequently proposed, hydroxylation, dehydrogenation, oxidation, N-oxidation, hydrolysis, reduction and glucuronide conjugation were mainly involved according to metabolic profile. The result proved application of this improved strategy was efficient, rapid, and reliable for metabolic profiling of components in multiple biological samples and could significantly expand our understanding of metabolic situation of TCM in vivo. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Electrostatic mass spectrometer for concurrent mass-, energy- and angle-resolved measurements

    International Nuclear Information System (INIS)

    Golikov, Yu.K.; Krasnova, N.K.

    1999-01-01

    A new electron-optical scheme is considered. An energy- and mass-analyser with angular resolution are combined in one device, in which a time-of-flight principle of mass separation is used. The tool is created on the basis of electrostatic field of quasi-conical systems possessing the high-energy dispersion and high-angular resolution. A regime of simultaneous angular and energy resolution is found. If there is an ion-pulsed source then the ion groups of equal mass will be registered at the same time at a position-sensitive detector located at the edge of the field. Real parameters of the suggested scheme are calculated

  3. Analysis of new psychoactive substances in human urine by ultra-high performance supercritical fluid and liquid chromatography: Validation and comparison.

    Science.gov (United States)

    Borovcová, Lucie; Pauk, Volodymyr; Lemr, Karel

    2018-05-01

    New psychoactive substances represent serious social and health problem as tens of new compounds are detected in Europe annually. They often show structural proximity or even isomerism, which complicates their analysis. Two methods based on ultra high performance supercritical fluid chromatography and ultra high performance liquid chromatography with mass spectrometric detection were validated and compared. A simple dilute-filter-and-shoot protocol utilizing propan-2-ol or methanol for supercritical fluid or liquid chromatography, respectively, was proposed to detect and quantify 15 cathinones and phenethylamines in human urine. Both methods offered fast separation (chromatography. Limits of detection in urine ranged from 0.01 to 2.3 ng/mL, except for cathinone (5 ng/mL) in supercritical fluid chromatography. Nevertheless, this technique distinguished all analytes including four pairs of isomers, while liquid chromatography was unable to resolve fluoromethcathinone regioisomers. Concerning matrix effects and recoveries, supercritical fluid chromatography produced more uniform results for different compounds and at different concentration levels. This work demonstrates the performance and reliability of supercritical fluid chromatography and corroborates its applicability as an alternative tool for analysis of new psychoactive substances in biological matrixes. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. On the Origin of Ultra High Energy Cosmic Rays II

    Energy Technology Data Exchange (ETDEWEB)

    Fowler, T K; Colgate, S; Li, H; Bulmer, R H; Pino, J

    2011-03-08

    We show that accretion disks around Active Galactic Nuclei (AGNs) could account for the enormous power in observed ultra high energy cosmic rays {approx}10{sup 20} eV (UHEs). In our model, cosmic rays are produced by quasi-steady acceleration of ions in magnetic structures previously proposed to explain jets around Active Galactic Nuclei with supermassive black holes. Steady acceleration requires that an AGN accretion disk act as a dynamo, which we show to follow from a modified Standard Model in which the magnetic torque of the dynamo replaces viscosity as the dominant mechanism accounting for angular momentum conservation during accretion. A black hole of mass M{sub BH} produces a steady dynamo voltage V {proportional_to} {radical}M{sub BH} giving V {approx} 10{sup 20} volts for M{sub BH} {approx} 10{sup 8} solar masses. The voltage V reappears as an inductive electric field at the advancing nose of a dynamo-driven jet, where plasma instability inherent in collisionless runaway acceleration allows ions to be steadily accelerated to energies {approx} V, finally ejected as cosmic rays. Transient events can produce much higher energies. The predicted disk radiation is similar to the Standard Model. Unique predictions concern the remarkable collimation of jets and emissions from the jet/radiolobe structure. Given MBH and the accretion rate, the model makes 7 predictions roughly consistent with data: (1) the jet length; (2) the jet radius; (3) the steady-state cosmic ray energy spectrum; (4) the maximum energy in this spectrum; (5) the UHE cosmic ray intensity on Earth; (6) electron synchrotron wavelengths; and (7) the power in synchrotron radiation. These qualitative successes motivate new computer simulations, experiments and data analysis to provide a quantitative verification of the model.

  5. Influence of Coulomb effects on the resolving power of multireflection mass-spectrometer systems

    International Nuclear Information System (INIS)

    Skoblin, M G; Kopaev, I A; Monastyrskiy, M A; Alimpiev, S S; Greenfield, D E; Makarov, A A

    2015-01-01

    General theoretical approaches to the modelling of Coulomb effects in short ion bunches, developed previously by the authors, are applied in this paper to the calculation of multireflection mass-spectrometer systems. A separate module of the MASIM 3D applied software package is designed. An adaptive computational procedure for calculating the 'mirror potential' induced by an ion bunch on the surface of field-forming electrodes is proposed. The dynamics of ion bunches in a time-of-flight reflectron-type mass analyser is calculated and the limitations on the resolving power, caused by resonant Coulomb effects of self-bunching and coalescence in the groups of particles with close masses, are revealed on the basis of numerical experiments. (laser applications and other topics in quantum electronics)

  6. Mass-dependent and non-mass-dependent isotope effects in ozone photolysis: Resolving theory and experiments

    International Nuclear Information System (INIS)

    Cole, Amanda S.; Boering, Kristie A.

    2006-01-01

    In addition to the anomalous 17 O and 18 O isotope effects in the three-body ozone formation reaction O+O 2 +M, isotope effects in the destruction of ozone by photolysis may also play a role in determining the isotopic composition of ozone and other trace gases in the atmosphere. While previous experiments on ozone photolysis at 254 nm were interpreted as evidence for preferential loss of light ozone that is anomalous (or 'non-mass-dependent'), recent semiempirical theoretical calculations predicted a preferential loss of heavy ozone at that wavelength that is mass dependent. Through photochemical modeling results presented here, we resolve this apparent contradiction between experiment and theory. Specifically, we show that the formation of ozone during the UV photolysis experiments is not negligible, as had been assumed, and that the well-known non-mass-dependent isotope effects in ozone formation can account for the non-mass-dependent enrichment of the heavy isotopologs of ozone observed in the experiment. Thus, no unusual non-mass-dependent fractionation in ozone photolysis must be invoked to explain the experimental results. Furthermore, we show that theoretical predictions of a mass-dependent preferential loss of the heavy isotopologs of ozone during UV photolysis are not inconsistent with the experimental data, particularly if mass-dependent isotope effects in the chemical loss reactions of ozone during the photolysis experiments or experimental artifacts enrich the remaining ozone in 17 O and 18 O. Before the calculated fractionation factors can be quantitatively evaluated, however, further investigation of possible mass-dependent isotope effects in the reactions of ozone with O( 1 D), O( 3 P), O 2 ( 1 Δ), and O 2 ( 1 Σ) is needed through experiments we suggest here

  7. Ultra-high-speed Optical Signal Processing using Silicon Photonics

    DEFF Research Database (Denmark)

    Oxenløwe, Leif Katsuo; Ji, Hua; Jensen, Asger Sellerup

    with a photonic layer on top to interconnect them. For such systems, silicon is an attractive candidate enabling both electronic and photonic control. For some network scenarios, it may be beneficial to use optical on-chip packet switching, and for high data-density environments one may take advantage...... of the ultra-fast nonlinear response of silicon photonic waveguides. These chips offer ultra-broadband wavelength operation, ultra-high timing resolution and ultra-fast response, and when used appropriately offer energy-efficient switching. In this presentation we review some all-optical functionalities based...... on silicon photonics. In particular we use nano-engineered silicon waveguides (nanowires) [1] enabling efficient phasematched four-wave mixing (FWM), cross-phase modulation (XPM) or self-phase modulation (SPM) for ultra-high-speed optical signal processing of ultra-high bit rate serial data signals. We show...

  8. Stretchers and compressors for ultra-high power laser systems

    Energy Technology Data Exchange (ETDEWEB)

    Yakovlev, I V [Institute of Applied Physics, Russian Academy of Sciences, Nizhnii Novgorod (Russian Federation)

    2014-05-30

    This review is concerned with pulse stretchers and compressors as key components of ultra-high power laser facilities that take advantage of chirped-pulse amplification. The potentialities, characteristics, configurations and methods for the matching and alignment of these devices are examined, with particular attention to the history of the optics of ultra-short, ultra-intense pulses before and after 1985, when the chirped-pulse amplification method was proposed, which drastically changed the view of the feasibility of creating ultra-high power laser sources. The review is intended primarily for young scientists and experts who begin to address the amplification and compression of chirped pulses, experts in laser optics and all who are interested in scientific achievements in the field of ultra-high power laser systems. (review)

  9. Angle resolved mass spectrometry of positive ions transmitted through high aspect ratio channels in a radio frequency discharge

    NARCIS (Netherlands)

    Stoffels - Adamowicz, E.; Stoffels, W.W.; Tachibana, K.; Imai, S.

    1997-01-01

    The behavior of positive ions in high aspect ratio structures, relevant to the reactive ion etching of deep trenches, has been studied by means of energy resolved mass spectrometry. High aspect ratio trenches are simulated by capillary plates with various aspect ratios. Angle resolved measurements

  10. Shock characterization of an ultra-high strength concrete

    International Nuclear Information System (INIS)

    Erzar, B.; Pontiroli, C.; Buzaud, E.

    2016-01-01

    Nowadays, the design of protective structures may imply ultra-high performance concretes. These materials present a compressive strength 5 times higher than standard concretes. However, few reliable data on the shock response of such materials are available in the literature. Thus, a characterization of an ultra-high strength concrete has been conducted by means of hydrostatic and triaxial tests in the quasi-static regime, and plate impact experiments for shock response. Data have been gathered up to 6 GPa and a simple modelling approach has been applied to get a reliable representation of the shock compression of this concrete. (authors)

  11. Scanning mass spectrometer setup for spatially resolved reactivity studies on model catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Roos, Matthias; Schirling, Christian; Kielbassa, Stefan; Bansmann, Joachim; Behm, Juergen [Institut fuer Oberflaechenchemie und Katalyse, Universitaet Ulm, D-89069 Ulm (Germany)

    2007-07-01

    A scanning mass spectrometer with micrometer-scale resolution was developed for investigations on the catalytic activity of microstructured planar model catalysts. Products of local surface reactions can be detected via a fine capillary orifice in a differentially pumped quadrupole mass spectrometer. The position of the sample with respect to the capillary is controlled by three piezo-driven translators. The surface reactivity of a resistive heated sample can be depicted in a spatially resolved topogram, taking into account the influence of the distance between sample and capillary on the magnitude of the QMS signal and the lateral resolution. Photolithographic structured reactive patterns on top of an inactive substrate enable investigations of mesoscopic transport effects such as coupling between catalytically active areas and of (reverse) spillover phenomena on one sample by varying the size and the distances of the active areas.

  12. Evaluation of a High Resolving Power Time-of-Flight Mass Spectrometer for Drug Analysis in Terms of Resolving Power and Acquisition Rate

    Science.gov (United States)

    Pelander, Anna; Decker, Petra; Baessmann, Carsten; Ojanperä, Ilkka

    2011-02-01

    Liquid chromatography time-of-flight mass spectrometry (LC-TOFMS) is applied increasingly to various fields of small molecule analysis. The moderate resolving power (RP) of standard TOFMS instruments poses a risk of false negative results when complex biological matrices are to be analyzed. In this study, the performance of a high resolving power TOFMS instrument (maXis by Bruker Daltonik, Bremen, Germany) was evaluated for drug analysis. By flow injection analysis of critical drug mixtures, including a total of 17 compounds with nominal masses of 212-415 Da and with mass differences of 8.8-23.5 mDa, RP varied from 34,400 to 51,900 (FWHM). The effect of acquisition rate on RP, mass accuracy, and isotopic pattern fit was studied by applying 1, 2, 5, 10, and 20 Hz acquisition rates in a 16 min gradient elution LC separation. All three variables were independent of the acquisition rate, with an average mass accuracy and isotopic pattern fit factor (mSigma) of 0.33 ppm and 5.9, respectively. The average relative standard deviation of RP was 1.8%, showing high repeatability. The performance was tested further with authentic urine extracts containing a co-eluting compound pair with a nominal mass of 296 Da and an 11.2 mDa mass difference. The authentic sample components were readily resolved and correctly identified by the automated data analysis. The average RP, mass accuracy, and isotopic pattern fit were 36,600, 0.9 ppm, and 7.3 mSigma, respectively.

  13. A High-mass Protobinary System with Spatially Resolved Circumstellar Accretion Disks and Circumbinary Disk

    Energy Technology Data Exchange (ETDEWEB)

    Kraus, S.; Kluska, J.; Kreplin, A.; Bate, M.; Harries, T. J.; Hone, E.; Anugu, A. [School of Physics, Astrophysics Group, University of Exeter, Stocker Road, Exeter EX4 4QL (United Kingdom); Hofmann, K.-H.; Weigelt, G. [Max-Planck-Institut für Radioastronomie, Auf dem Hügel 69, D-53121 Bonn (Germany); Monnier, J. D. [Department of Astronomy, University of Michigan, 311 West Hall, 1085 South University Avenue, Ann Arbor, MI 48109 (United States); De Wit, W. J. [ESO, Alonso de Cordova 3107, Vitacura, Santiago 19 (Chile); Wittkowski, M., E-mail: skraus@astro.ex.ac.uk [ESO, Karl-Schwarzschild-Str. 2, D-85748 Garching bei München (Germany)

    2017-01-20

    High-mass multiples might form via fragmentation of self-gravitational disks or alternative scenarios such as disk-assisted capture. However, only a few observational constraints exist on the architecture and disk structure of high-mass protobinaries and their accretion properties. Here, we report the discovery of a close (57.9 ± 0.2 mas = 170 au) high-mass protobinary, IRAS17216-3801, where our VLTI/GRAVITY+AMBER near-infrared interferometry allows us to image the circumstellar disks around the individual components with ∼3 mas resolution. We estimate the component masses to ∼20 and ∼18 M {sub ⊙} and find that the radial intensity profiles can be reproduced with an irradiated disk model, where the inner regions are excavated of dust, likely tracing the dust sublimation region in these disks. The circumstellar disks are strongly misaligned with respect to the binary separation vector, which indicates that the tidal forces did not have time to realign the disks, pointing toward a young dynamical age of the system. We constrain the distribution of the Br γ and CO-emitting gas using VLTI/GRAVITY spectro-interferometry and VLT/CRIRES spectro-astrometry and find that the secondary is accreting at a higher rate than the primary. VLT/NACO imaging shows L ′-band emission on (3–4)× larger scales than the binary separation, matching the expected dynamical truncation radius for the circumbinary disk. The IRAS17216-3801 system is ∼3× more massive and ∼5× more compact than other high-mass multiplies imaged at infrared wavelength and the first high-mass protobinary system where circumstellar and circumbinary dust disks could be spatially resolved. This opens exciting new opportunities for studying star–disk interactions and the role of multiplicity in high-mass star formation.

  14. Comparison of ultra-high performance supercritical fluid chromatography and ultra-high performance liquid chromatography for the separation of spirostanol saponins.

    Science.gov (United States)

    Zhu, Ling-Ling; Zhao, Yang; Xu, Yong-Wei; Sun, Qing-Long; Sun, Xin-Guang; Kang, Li-Ping; Yan, Ren-Yi; Zhang, Jie; Liu, Chao; Ma, Bai-Ping

    2016-02-20

    Spirostanol saponins are important active components of some herb medicines, and their isolation and purification are crucial for the research and development of traditional Chinese medicines. We aimed to compare the separation of spirostanol saponins by ultra-high performance supercritical fluid chromatography (UHPSFC) and ultra-high performance liquid chromatography (UHPLC). Four groups of spirostanol saponins were separated respectively by UHPSFC and UHPLC. After optimization, UHPSFC was performed with a HSS C18 SB column or a Diol column and with methanol as the co-solvent. A BEH C18 column and mobile phase containing water (with 0.1% formic acid) and acetonitrile were used in UHPLC. We found that UHPSFC could be performed automatically and quickly. It is effective in separating the spirostanol saponins which share the same aglycone and vary in sugar chains, and is very sensitive to the number and the position of hydroxyl groups in aglycones. However, the resolution of spirostanol saponins with different aglycones and the same sugar moiety by UHPSFC was not ideal and could be resolved by UHPLC instead. UHPLC is good at differentiating the variation in aglycones, and is influenced by double bonds in aglycones. Therefore, UHPLC and UHPSFC are complementary in separating spirostanol saponins. Considering the naturally produced spirostanol saponins in herb medicines are different both in aglycones and in sugar chains, a better separation can be achieved by combination of UHPLC and UHPSFC. UHPSFC is a powerful technique for improving the resolution when UHPLC cannot resolve a mixture of spirostanol saponins and vice versa. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Status of Ultra-High Energy Cosmic Rays

    CERN Multimedia

    CERN. Geneva

    2015-01-01

    I will review the recent results on Ultra-High energy cosmic rays obtained by the Auger and Telescope Array Observatories, and discuss some of the Astrophysical scenarios that could account for them, a connection with LHC results  as well as the possible connections to neutrino and gamma ray observations.

  16. Soliton-based ultra-high speed optical communications

    Indian Academy of Sciences (India)

    All these facts are the outcome of research on optical solitons in fibers in spite of the fact that the commonly used RZ format is not always called a soliton format. The overview presented here attempts to incorporate the role of soliton-based communications research in present day ultra-high speed communications.

  17. Influence of curing regimes on compressive strength of ultra high

    Indian Academy of Sciences (India)

    The present paper is aimed to identify an efficient curing regime for ultra high performance concrete (UHPC), to achieve a target compressive strength more than 150 MPa, using indigenous materials. The thermal regime plays a vital role due to the limited fineness of ingredients and low water/binder ratio. By activation of the ...

  18. Ultra high performance liquid chromatography of seized drugs

    NARCIS (Netherlands)

    Lurie, I.S.

    2010-01-01

    The primary goal of this thesis is to investigate the use of ultra high performance liquid chromatography (UHPLC) for the analysis of seized drugs. This goal was largely achieved and significant progress was made in achieving improved separation and detection of drugs of forensic interest.

  19. Ultra high energy cosmic rays and magnetic fields

    Energy Technology Data Exchange (ETDEWEB)

    Stanev, Todor; Engel, Ralph; Alvarez-Muniz, Jaime; Seckel, David

    2002-07-01

    We follow the propagation of ultra high energy protons in the presence of random and regular magnetic fields and discuss some of the changes in the angular and energy distributions of these particles introduced by the scattering in the magnetic fields.

  20. Ultra high energy cosmic rays and magnetic fields

    International Nuclear Information System (INIS)

    Stanev, Todor; Engel, Ralph; Alvarez-Muniz, Jaime; Seckel, David

    2002-01-01

    We follow the propagation of ultra high energy protons in the presence of random and regular magnetic fields and discuss some of the changes in the angular and energy distributions of these particles introduced by the scattering in the magnetic fields

  1. Fiber based hydrophones for ultra-high energy neutrino detection

    NARCIS (Netherlands)

    Buis, E.J.; Doppenberg, E.J.J.; Eijk, D. van; Lahmann, R.; Nieuwland, R.A.; Toet, P.M.

    2014-01-01

    It is a well studied process [1, 2] that energy deposition of cosmic ray particles in water that generate thermo-acoustic signals. Hydrophones of sufficient sensitivity could measure this signal and provide a means of detecting ultra-high energetic cosmic neutrinos. We investigate optical

  2. Super Boiler: First Generation, Ultra-High Efficiency Firetube Boiler

    Energy Technology Data Exchange (ETDEWEB)

    None

    2006-06-01

    This factsheet describes a research project whose goal is to develop and demonstrate a first-generation ultra-high-efficiency, ultra-low emissions, compact gas-fired package boiler (Super Boiler), and formulate a long-range RD&D plan for advanced boiler technology out to the year 2020.

  3. Construction, characterization and applications of a compact mass-resolved low-energy ion beam system

    International Nuclear Information System (INIS)

    Lau, W.M.; Feng, X.; Bello, I.; Sant, S.; Foo, K.K.; Lawson, R.P.W.

    1991-01-01

    A compact mass-resolved low-energy ion beam system has been constructed in which ions are extracted from a Colutron ion source, focused by an einzel lens, mass-selected by a Wien filter, refocused by a second einzel lens into an ultrahigh vacuum target chamber, and finally decelerated with a five-electrode lens. The design of the deceleration lens was assisted by computer simulation including space-charge effects with an ion trajectory software (CHDEN). The system performance has been characterized with a quadrupole mass spectrometer and an energy analyzer along the beam axis. For example, argon ions can be transported at keV and decelerated to 10 eV with an energy spread of ±0.5 eV. The total current measured by a Faraday cage at the exit of the deceleration lens in the energy range of 10-200 eV is about 1-5 μA. The ion current density was higher than 100 μA/cm 2 at 50 eV but decreased to 10-20 μA/cm 2 at 10 eV. The mass resolution was estimated to be 40 under the present operation configuration. The system has been used to produce interesting results in both ion beam etching and deposition. (orig.)

  4. Ultra-high performance liquid chromatography coupled with photo-diode array and quadrupole/time-of-flight mass spectrometry based chemical profiling approach to evaluate the influence of preparation methods on the holistic quality of Qiong-Yu-Gao, a traditional complex herbal medicine.

    Science.gov (United States)

    Xu, Jin-Di; Mao, Qian; Shen, Hong; Zhu, Ling-Ying; Li, Song-Lin; Yan, Ru

    2013-08-23

    Qiong-Yu-Gao (QYG), consisting of Rehmanniae Radix (RR), Poriae (PO) and Ginseng Radix (GR), is a commonly used tonic traditional complex herbal medicine (CHM). So far, three different methods have been documented for preparation of QYG, i.e. method 1 (M1): mixing powders of GR and PO with decoction of RR; method 2 (M2): combining the decoction of RR and PO with the decoction of GR; method 3 (M3): decocting the mixture of RR, GR and PO. In present study, an ultra-high performance liquid chromatography coupled with photo-diode array and quadrupole/time-of-flight mass spectrometry (UHPLC-PDA-QTOF-MS/MS) based chemical profiling approach was developed to investigate the influence of the three preparation methods on the holistic quality of QYG. All detected peaks were unambiguously identified by comparing UV spectra, accurate mass data/characteristic mass fragments and retention times with those of reference compounds, and/or tentatively assigned by matching empirical molecular formula with that of known compounds, and/or elucidating quasi-molecular ions and fragment ions referring to information available in literature. A total of 103 components, mainly belonging to ginsenosides, phenethylalcohol glycosides, iridoid glycosides and triterpenoid acids, were identified, of which 5 degraded ginsenosides were putatively determined to be newly generated during preparation procedures of QYG samples. Triterpenoid acids and malonyl-ginsenosides were detected only in M1 samples, while degraded ginsenosides were merely detectable in M2/M3 samples. The possible reasons for the difference among chemical profiles of QYG samples prepared with three methods were also discussed. It could be concluded that preparation method do significantly affect the holistic quality of QYG. The influence of the altered chemical profiles on the bioactivity of QYG needs further investigation. The present study demonstrated that UHPLC-PDA-QTOF-MS/MS based chemical profiling approach is efficient and

  5. High mass accuracy and high mass resolving power FT-ICR secondary ion mass spectrometry for biological tissue imaging

    NARCIS (Netherlands)

    Smith, D.F.; Kiss, A.; Leach, F.E.; Robinson, E.W.; Paša-Tolić, L.; Heeren, R.M.A.

    2013-01-01

    Biological tissue imaging by secondary ion mass spectrometry has seen rapid development with the commercial availability of polyatomic primary ion sources. Endogenous lipids and other small bio-molecules can now be routinely mapped on the sub-micrometer scale. Such experiments are typically

  6. THE PANCHROMATIC HUBBLE ANDROMEDA TREASURY. III. MEASURING AGES AND MASSES OF PARTIALLY RESOLVED STELLAR CLUSTERS

    Energy Technology Data Exchange (ETDEWEB)

    Beerman, Lori C.; Johnson, L. Clifton; Fouesneau, Morgan; Dalcanton, Julianne J.; Weisz, Daniel R.; Williams, Ben F. [Department of Astronomy, University of Washington, Box 351580, Seattle, WA 98195 (United States); Seth, Anil C. [Department of Physics and Astronomy, University of Utah, Salt Lake City, UT 84112 (United States); Bell, Eric F. [Department of Astronomy, University of Michigan, 500 Church Street, Ann Arbor, MI 48109 (United States); Bianchi, Luciana C. [Department of Physics and Astronomy, Johns Hopkins University, 3400 North Charles Street, Baltimore, MD 21218 (United States); Caldwell, Nelson [Harvard-Smithsonian Center for Astrophysics, 60 Garden Street, Cambridge, MA 02138 (United States); Dolphin, Andrew E. [Raytheon Company, 1151 East Hermans Road, Tucson, AZ 85756 (United States); Gouliermis, Dimitrios A. [Zentrum fuer Astronomie, Institut fuer Theoretische Astrophysik, Universitaet Heidelberg, Albert-Ueberle-Strasse 2, D-69120 Heidelberg (Germany); Kalirai, Jason S. [Space Telescope Science Institute, 3700 San Martin Drive, Baltimore, MD 21218 (United States); Larsen, Soren S. [Department of Astrophysics, IMAPP, Radboud University Nijmegen, P.O. Box 9010, NL-6500 GL Nijmegen (Netherlands); Melbourne, Jason L. [Caltech Optical Observatories, Division of Physics, Mathematics and Astronomy, Mail Stop 301-17, California Institute of Technology, Pasadena, CA 91125 (United States); Rix, Hans-Walter [Max-Planck-Institut fuer Astronomie, Koenigstuhl 17, D-69117 Heidelberg (Germany); Skillman, Evan D., E-mail: beermalc@astro.washington.edu [Department of Astronomy, University of Minnesota, 116 Church Street SE, Minneapolis, MN 55455 (United States)

    2012-12-01

    The apparent age and mass of a stellar cluster can be strongly affected by stochastic sampling of the stellar initial mass function (IMF), when inferred from the integrated color of low-mass clusters ({approx}<10{sup 4} M {sub Sun }). We use simulated star clusters to show that these effects are minimized when the brightest, rapidly evolving stars in a cluster can be resolved, and the light of the fainter, more numerous unresolved stars can be analyzed separately. When comparing the light from the less luminous cluster members to models of unresolved light, more accurate age estimates can be obtained than when analyzing the integrated light from the entire cluster under the assumption that the IMF is fully populated. We show the success of this technique first using simulated clusters, and then with a stellar cluster in M31. This method represents one way of accounting for the discrete, stochastic sampling of the stellar IMF in less massive clusters and can be leveraged in studies of clusters throughout the Local Group and other nearby galaxies.

  7. Angular and mass resolved energy distribution measurements with a gallium liquid metal ion source

    International Nuclear Information System (INIS)

    Marriott, Philip

    1987-06-01

    Ionisation and energy broadening mechanisms relevant to liquid metal ion sources are discussed. A review of experimental results giving a picture of source operation and a discussion of the emission mechanisms thought to occur for the ionic species and droplets emitted is presented. Further work is suggested by this review and an analysis system for angular and mass resolved energy distribution measurements of liquid metal ion source beams has been constructed. The energy analyser has been calibrated and a series of measurements, both on and off the beam axis, of 69 Ga + , Ga ++ and Ga 2 + ions emitted at various currents from a gallium source has been performed. A comparison is made between these results and published work where possible, and the results are discussed with the aim of determining the emission and energy spread mechanisms operating in the gallium liquid metal ion source. (author)

  8. Motivation for an SSC detector with ultra-high resolution photon detection

    International Nuclear Information System (INIS)

    Gunion, J.F.; Kane, G.

    1992-01-01

    It is well known that incorporating ultra-high resolution photon detection into a general purpose detector for the SSC will be extremely difficult. The authors will argue that the physics signals that could be missed without such resolution are of such importance that a special purpose detector designed specifically for photon final state modes should be constructed, if sufficient resolution cannot be achieved with general purpose detectors. The potentially great value of these signals as a probe of extremely high mass scales is stressed

  9. Mass measurement of cooled neutron-deficient bismuth projectile fragments with time-resolved Schottky mass spectrometry at the FRS-ESR facility

    Energy Technology Data Exchange (ETDEWEB)

    Litvinov, Yu.A.; Geissel, H. [Giessen Univ. (Germany); Radon, T. [Gesellschaft fuer Schwerionenforschung mbH, Darmstadt (DE)] [and others

    2005-06-01

    Masses of 582 neutron-deficient nuclides (30{<=}Z{<=}85) were measured with time-resolved Schottky mass spectrometry at the FRS-ESR facility at GSI, 117 were used for calibration. The masses of 71 nuclides were obtained for the first time. A typical mass accuracy of 30 {mu}u was achieved. These data have entered the latest atomic mass evaluation. The mass determination of about 140 additional nuclides was possible via known energies (Q-values) of {alpha}-, {beta}-, or proton decays. The obtained results are compared with the results of other measurements. (orig.)

  10. Modification of Ultra-High Vacuum Surfaces Using Free Radicals

    CERN Document Server

    Vorlaufer, G

    2002-01-01

    In ultra-high vacuum systems outgassing from vacuum chamber walls and desorption of surface adsorbates are usually the factors which determine pressure and residual gas composition. In particular in beam vacuum systems of accelerators like the LHC, where surfaces are exposed to intense synchrotron radiation and bombardment by energetic ions and electrons, surface properties like the molecular desorption yield or secondary electron yield can strongly influence the performance of the accelerator. Well-established treatment methods like vacuum bake-out or glow-discharge cleaning have been successfully applied in the past to condition ultra-high vacuum surfaces, but these methods are sometimes difficult to carry out, for example if the vacuum chambers are not accessible. In this work, an alternative treatment method is investigated. This method is based on the strong chemical reactivity of free radicals, electrically neutral fragments of molecules. Free radicals (in the case of this work, nitrogen and oxygen radi...

  11. Functional aluminum alloys for ultra high vacuum use

    International Nuclear Information System (INIS)

    Kato, Yutaka; Tsukamoto, Kenji; Isoyama, Eizo

    1985-01-01

    Ultra high vacuum systems made of aluminum alloys are actively developed. The reasons for using aluminum alloys are low residual radioactivity, light weight, good machinability, good thermal conductivity, non-magnetism. The important function required for ultra high vacuum materials is low outgassing rate, but surface gas on ordinary aluminum is much. Then the research on aluminum surface structure with low outgassing rate has been made and the special extrusion method, that is, extrusion method with the conditions of preventing air from entering inside of pipe and of taking in mixture gas of Ar + O 2 , was developed. 6063 alloy obtained by special extrusion method showed low outgassing rate (2 x 10 -13 Torr. 1/s. cm 2 ) by only 150 deg C, 24 h baking. For the future it will be important to develop aluminum alloys with low dynamic outgassing rate as well as low static outgassing rate. (author)

  12. Resolving the neutrino mass hierarchy and CP degeneracy by two identical detectors with different baselines

    International Nuclear Information System (INIS)

    Ishitsuka, Masaki; Kajita, Takaaki; Minakata, Hisakazu; Nunokawa, Hiroshi

    2005-01-01

    We explore the possibility of the simultaneous determination of neutrino mass hierarchy and the CP violating phase by using two identical detectors placed at different baseline distances. We focus on a possible experimental setup using a neutrino beam from the J-PARC facility in Japan with a beam power of 4 MW and megaton (Mton)-class water Cherenkov detectors, one placed in Kamioka and the other somewhere in Korea. We demonstrate, under reasonable assumptions of systematic uncertainties, that the two-detector complex with each fiducial volume of 0.27 Mton has a potential of resolving the neutrino mass hierarchy up to sin 2 2θ 13 >0.03 (0.055) at 2σ (3σ) C.L. for any values of δ and at the same time has the sensitivity to CP violation by 4+4 years running of ν e and ν e appearance measurement. The significantly enhanced sensitivity is due to clean detection of the modulation of the neutrino energy spectrum, which is enabled by the cancellation of systematic uncertainties between two identical detectors which receive the neutrino beam with the same energy spectrum in the absence of oscillations

  13. Ultra high frequency induction welding of powder metal compacts

    Energy Technology Data Exchange (ETDEWEB)

    Cavdar, U.; Gulsahin, I.

    2014-10-01

    The application of the iron based Powder Metal (PM) compacts in Ultra High Frequency Induction Welding (UHFIW) were reviewed. These PM compacts are used to produce cogs. This study investigates the methods of joining PM materials enforceability with UHFIW in the industry application. Maximum stress and maximum strain of welded PM compacts were determined by three point bending and strength tests. Microhardness and microstructure of induction welded compacts were determined. (Author)

  14. Ultra high frequency induction welding of powder metal compacts

    International Nuclear Information System (INIS)

    Cavdar, U.; Gulsahin, I.

    2014-01-01

    The application of the iron based Powder Metal (PM) compacts in Ultra High Frequency Induction Welding (UHFIW) were reviewed. These PM compacts are used to produce cogs. This study investigates the methods of joining PM materials enforceability with UHFIW in the industry application. Maximum stress and maximum strain of welded PM compacts were determined by three point bending and strength tests. Microhardness and microstructure of induction welded compacts were determined. (Author)

  15. Ultra-high-field magnets for future hadron colliders

    International Nuclear Information System (INIS)

    McIntyre, P.M.; Shen, W.

    1997-01-01

    Several new concepts in magnetic design and coil fabrication are being incorporated into designs for ultra-high field collider magnets: a 16 Tesla block-coil dual dipole, also using Nb 3 Sn cable, featuring simple pancake coil construction and face-loaded prestress geometry; a 330 T/m block-coil quadrupole; and a ∼ 20 Tesla pipe-geometry dual dipole, using A15 or BSCCO tape. Field design and fabrication issues are discussed for each magnet

  16. Ultra-high energy cosmic rays: Setting the stage

    Science.gov (United States)

    Sokolsky, P.

    2013-06-01

    The history of ultra-high energy cosmic ray physics is reviewed from the post-war era of arrays such as Volcano Ranch, Haverah Park and Akeno to the development of air-fluorescence and current hybrid arrays. The aim of this paper is to present the background information needed for a better understanding of the current issues in this field that are discussed in much greater depth in the rest of this conference.

  17. Ultra-high energy cosmic rays: Setting the stage

    Directory of Open Access Journals (Sweden)

    Sokolsky P.

    2013-06-01

    Full Text Available The history of ultra-high energy cosmic ray physics is reviewed from the post-war era of arrays such as Volcano Ranch, Haverah Park and Akeno to the development of air-fluorescence and current hybrid arrays. The aim of this paper is to present the background information needed for a better understanding of the current issues in this field that are discussed in much greater depth in the rest of this conference.

  18. A swimming pool array for ultra high energy showers

    Science.gov (United States)

    Yodh, Gaurang B.; Shoup, Anthony; Barwick, Steve; Goodman, Jordan A.

    1992-11-01

    A very preliminary design concept for an array using water Cherenkov counters, built out of commercially available backyard swimming pools, to sample the electromagnetic and muonic components of ultra high energy showers at large lateral distances is presented. The expected performance of the pools is estimated using the observed lateral distributions by scintillator and water Cherenkov arrays at energies above 1019 eV and simulations.

  19. Ultra-high Performance Liquid Chromatography in Steroid Analysis

    OpenAIRE

    Salonen, Fanny

    2017-01-01

    The latest version of liquid chromatography is ultra-high performance (or pressure) chromatography (UHPLC). In the technique, short and narrow-bore columns with particle sizes below 3 µm are used. The extremely high pressure used results in very short analysis times, excellent separation, and good resolution. This makes UHPLC a good choice for steroidal analysis. Steroids are a highly interesting area of study; they can be recognized as biomarkers for several diseases and are a relevant topic...

  20. Recent Ultra High Energy neutrino bounds and multimessenger observations with the Pierre Auger Observatory

    Science.gov (United States)

    Zas, Enrique

    2018-01-01

    The overall picture of the highest energy particles produced in the Universe is changing because of measurements made with the Pierre Auger Observatory. Composition studies of cosmic rays point towards an unexpected mixed composition of intermediate mass nuclei, more isotropic than anticipated, which is reshaping the future of the field and underlining the priority to understand composition at the highest energies. The Observatory is competitive in the search for neutrinos of all flavors above about 100 PeV by looking for very inclined showers produced deep in the atmosphere by neutrinos interacting either in the atmosphere or in the Earth's crust. It covers a large field of view between -85° and 60° declination in equatorial coordinates. Neutrinos are expected because of the existence of ultra high energy cosmic rays. They provide valuable complementary information, their fluxes being sensitive to the primary cosmic ray masses and their directions reflecting the source positions. We report the results of the neutrino search providing competitive bounds to neutrino production and strong constraints to a number of production models including cosmogenic neutrinos due to ultra high energy protons. We also report on two recent contributions of the Observatory to multimessenger studies by searching for correlations of neutrinos both with cosmic rays and with gravitational waves. The correlations of the directions of the highest energy astrophysical neutrinos discovered with IceCube with the highest energy cosmic rays detected with the Auger Observatory and the Telescope Array revealed an excess that is not statistically significant and is being monitored. The targeted search for neutrinos correlated with the discovery of the gravitational wave events GW150914 and GW151226 with advanced LIGO has led to the first bounds on the energy emitted by black hole mergers in Ultra-High Energy Neutrinos.

  1. Recent Ultra High Energy neutrino bounds and multimessenger observations with the Pierre Auger Observatory

    Directory of Open Access Journals (Sweden)

    Zas Enrique

    2017-01-01

    Full Text Available The overall picture of the highest energy particles produced in the Universe is changing because of measurements made with the Pierre Auger Observatory. Composition studies of cosmic rays point towards an unexpected mixed composition of intermediate mass nuclei, more isotropic than anticipated, which is reshaping the future of the field and underlining the priority to understand composition at the highest energies. The Observatory is competitive in the search for neutrinos of all flavors above about 100 PeV by looking for very inclined showers produced deep in the atmosphere by neutrinos interacting either in the atmosphere or in the Earth’s crust. It covers a large field of view between −85◦ and 60◦ declination in equatorial coordinates. Neutrinos are expected because of the existence of ultra high energy cosmic rays. They provide valuable complementary information, their fluxes being sensitive to the primary cosmic ray masses and their directions reflecting the source positions. We report the results of the neutrino search providing competitive bounds to neutrino production and strong constraints to a number of production models including cosmogenic neutrinos due to ultra high energy protons. We also report on two recent contributions of the Observatory to multimessenger studies by searching for correlations of neutrinos both with cosmic rays and with gravitational waves. The correlations of the directions of the highest energy astrophysical neutrinos discovered with IceCube with the highest energy cosmic rays detected with the Auger Observatory and the Telescope Array revealed an excess that is not statistically significant and is being monitored. The targeted search for neutrinos correlated with the discovery of the gravitational wave events GW150914 and GW151226 with advanced LIGO has led to the first bounds on the energy emitted by black hole mergers in Ultra-High Energy Neutrinos.

  2. Simultaneous determination and qualitative analysis of six types of components in Naoxintong capsule by miniaturized matrix solid-phase dispersion extraction coupled with ultra high-performance liquid chromatography with photodiode array detection and quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Wang, Huilin; Jiang, Yan; Ding, Mingya; Li, Jin; Hao, Jia; He, Jun; Wang, Hui; Gao, Xiu-Mei; Chang, Yan-Xu

    2018-02-03

    A simple and effective sample preparation process based on miniaturized matrix solid-phase dispersion was developed for simultaneous determination of phenolic acids (gallic acid, chlorogenic acid, ferulic acid, 3,5-dicaffeoylqunic acid, 1,5-dicaffeoylqunic acid, rosmarinic acid, lithospermic acid, and salvianolic acid B), flavonoids (kaempferol-3-O-rutinoside, calycosin, and formononetin), lactones (ligustilide and butyllidephthalide), monoterpenoids (paeoniflorin), phenanthraquinones (cryptotanshinone), and furans (5-hydroxymethylfurfural) in Naoxintong capsule by ultra high-performance liquid chromatography. The optimized condition was that 25 mg Naoxintong powder was blended homogeneously with 100 mg Florisil PR for 4 min. One milliliter of methanol/water (75:25, v/v) acidified by 0.05% formic acid was selected to elute all components. It was found that the recoveries of the six types of components ranged from 61.36 to 96.94%. The proposed miniaturized matrix solid-phase dispersion coupled with ultra high-performance liquid chromatography was successfully applied to simultaneous determination of the six types of components in Naoxintong capsules. The results demonstrated that the proposed miniaturized matrix solid-phase dispersion coupled with ultra high-performance liquid chromatography could be used as an environmentally friendly tool for the extraction and determination of multiple bioactive components in natural products. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Ultra-high vacuum compatible optical chopper system for synchrotron x-ray scanning tunneling microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Chang, Hao, E-mail: hc000211@ohio.edu [Advanced Photon Source, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439 (United States); Nanoscale and Quantum Phenomena Institute, Physics & Astronomy Department, Ohio University, Athens, Ohio 45701 (United States); Cummings, Marvin; Shirato, Nozomi; Stripe, Benjamin; Preissner, Curt; Freeland, John W. [Advanced Photon Source, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439 (United States); Rosenmann, Daniel [Center for Nanoscale Materials, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439 (United States); Kersell, Heath; Hla, Saw-Wai [Nanoscale and Quantum Phenomena Institute, Physics & Astronomy Department, Ohio University, Athens, Ohio 45701 (United States); Center for Nanoscale Materials, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439 (United States); Rose, Volker, E-mail: vrose@anl.gov [Advanced Photon Source, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439 (United States); Center for Nanoscale Materials, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439 (United States)

    2016-01-28

    High-speed beam choppers are a crucial part of time-resolved x-ray studies as well as a necessary component to enable elemental contrast in synchrotron x-ray scanning tunneling microscopy (SX-STM). However, many chopper systems are not capable of operation in vacuum, which restricts their application to x-ray studies with high photon energies, where air absorption does not present a significant problem. To overcome this limitation, we present a fully ultra-high vacuum (UHV) compatible chopper system capable of operating at variable chopping frequencies up to 4 kHz. The lightweight aluminum chopper disk is coated with Ti and Au films to provide the required beam attenuation for soft and hard x-rays with photon energies up to about 12 keV. The chopper is used for lock-in detection of x-ray enhanced signals in SX-STM.

  4. Compact Starburst Galaxies with Fast Outflows: Spatially Resolved Stellar Mass Profiles

    Science.gov (United States)

    Gottlieb, Sophia; Diamond-Stanic, Aleksandar; Lipscomb, Charles; Ohene, Senyo; Rines, Josh; Moustakas, John; Sell, Paul; Tremonti, Christy; Coil, Alison; Rudnick, Gregory; Hickox, Ryan C.; Geach, James; Kepley, Amanda

    2018-01-01

    Powerful galactic winds driven by stellar feedback and black hole accretion are thought to play an important role in regulating star formation in galaxies. In particular, strong stellar feedback from supernovae, stellar winds, radiation pressure, and cosmic rays is required by simulations of star-forming galaxies to prevent the vast majority of baryons from cooling and collapsing to form stars. However, it remains unclear whether these stellar processes play a significant role in expelling gas and shutting down star formation in massive progenitors of quiescent galaxies. What are the limits of stellar feedback? We present multi-band photometry with HST/WFC3 (F475W, F814W, F160W) for a dozen compact starburst galaxies at z~0.6 with half-light radii that suggest incredibly large central escape velocities. These massive galaxies are driving fast (>1000 km/s) outflows that have been previously attributed to stellar feedback associated with the compact (r~100 pc) starburst. But how compact is the stellar mass? In the context of the stellar feedback hypothesis, it is unclear whether these fast outflows are being driven at velocities comparable to the escape velocity of an incredibly dense stellar system (as predicted by some models of radiation-pressure winds) or at velocities that exceed the central escape velocity by large factor. Our spatially resolved measurements with HST show that the stellar mass is more extended than the light, and this requires that the physical mechanism responsible for driving the winds must be able to launch gas at velocities that are factors of 5-10 beyond the central escape velocity.

  5. Phase-Resolved Spectroscopy of the Low-Mass X-ray Binary V801 Ara

    Science.gov (United States)

    Brauer, Kaley; Vrtilek, Saeqa Dil; Peris, Charith; McCollough, Michael

    2018-06-01

    We present phase-resolved optical spectra of the low mass X-ray binary system V801 Ara. The spectra, obtained in 2014 with IMACS on the Magellan/Baade telescope at Las Campanas Observatory, cover the full binary orbit of 3.8 hours. They contain strong emission features allowing us to map the emission of Hα, Hβ, He II λ4686, and the Bowen blend at λ4640. The radial velocity curves of the Bowen blend shows significantly stronger modulation at the orbital period than Hα as expected for the former originating on the secondary with the latter consistent with emission dominated by the disk. Our tomograms of Hα and Hβ are the most detailed studies of these lines for V801 to date and they clearly detect the accretion disk. The Hβ emission extends to higher velocities than Hα, suggesting emission from closer to the neutron star and differentiating temperature variance in the accretion disk for the first time. The center of the accretion disk appears offset from the center-of-mass of the neutron star as has been seen in several other X-ray binaries. This is often interpreted to imply disk eccentricity. Our tomograms do not show strong evidence for a hot spot at the point where the accretion stream hits the disk. This could imply a reduced accretion rate or could be due to the spot being drowned out by bright accretion flow around it. There is enhanced emission further along the disk, however, which implies gas stream interaction downstream of the hot spot.

  6. ATLAS and ultra high energy cosmic ray physics

    Directory of Open Access Journals (Sweden)

    Pinfold James

    2017-01-01

    Full Text Available After a brief introduction to extended air shower cosmic ray physics the current and future deployment of forward detectors at ATLAS is discussed along with the various aspects of the current and future ATLAS programs to explore hadronic physics. The emphasis is placed on those results and future plans that have particular relevance for high-energy, and ultra high-energy, cosmic ray physics. The possible use of ATLAS as an “underground” cosmic muon observatory is briefly considered.

  7. Functional magnetic resonance imaging with ultra-high fields

    International Nuclear Information System (INIS)

    Windischberger, C.; Schoepf, V.; Sladky, R.; Moser, E.; Fischmeister, F.P.S.

    2010-01-01

    Functional magnetic resonance imaging (fMRI) is currently the primary method for non-invasive functional localization in the brain. With the emergence of MR systems with field strengths of 4 Tesla and above, neuronal activation may be studied with unprecedented accuracy. In this article we present different approaches to use the improved sensitivity and specificity for expanding current fMRT resolution limits in space and time based on several 7 Tesla studies. In addition to the challenges that arise with ultra-high magnetic fields possible solutions will be discussed. (orig.) [de

  8. Photonic Technologies for Ultra-High-Speed Information Highways

    DEFF Research Database (Denmark)

    Bouchoule, S; Lèfevre, R.; Legros, E.

    1999-01-01

    The ACTS project HIGHWAY (AC067) addresses promising ultra-high speed optoelectronic components and system technologies for 40 Gbit/s time-division-multiplexed (TDM) transport systems. Advanced 40 Gbit/s TDM system lab demonstrators are to be realized and tested over installed field fiber testbeds....... This paper reviews the current status of 40 Gbit/s TDM components and subsystem technologies achieved in HIGHWAY. The results of HIGHWAY 40 Gbit/s TDM systems and field tests will be reported in a subsequent paper. (C) 1999 Academic Press....

  9. Design of Ultra High Performance Fiber Reinforced Concrete Shells

    DEFF Research Database (Denmark)

    Jepsen, Michael S.; Lambertsen, Søren Heide; Damkilde, Lars

    2013-01-01

    Fiber Reinforced Concrete shell. The major challenge in the design phase has been securing sufficient stiffness of the structure while keeping the weight at a minimum. The weight/stiffness issue has been investigated by means of the finite element method, to optimize the structure regarding overall......The paper treats the redesign of the float structure of the Wavestar wave energy converter. Previously it was designed as a glass fiber structure, but due to cost reduction requirements a redesign has been initiated. The new float structure will be designed as a double curved Ultra High Performance...

  10. The influence of the observatory latitude on the study of ultra high energy cosmic rays

    Energy Technology Data Exchange (ETDEWEB)

    Anjos, Rita C. dos [Departamento de Engenharias e Exatas, Universidade Federal do Paraná (UFPR), Pioneiro, 2153, Palotina, PR, 85950-000 Brazil (Brazil); De Souza, Vitor [Instituto de Física de São Carlos, Universidade de São Paulo, CP 369, São Carlos, SP, 13560-970 Brazil (Brazil); De Almeida, Rogerio M. [EEIMVR, Universidade Federal Fluminense, Volta Redonda, RJ (Brazil); Santos, Edivaldo M., E-mail: ritacassia@ufpr.br, E-mail: vitor@ifsc.usp.br, E-mail: rmenezes@id.uff.br, E-mail: emoura@if.usp.br [Instituto de Física, Universidade de São Paulo, Rua do Matão trav. R 187, São Paulo, 05508-090 Brazil (Brazil)

    2017-07-01

    Recent precision measurements of the Ultra High Energy Cosmic Rays (UHECR) arrival directions, spectrum and parameters related to the mass of the primary particle have been done by the HiRes, Pierre Auger and Telescope Array (TA) Observatories. In this paper, distributions of arrival directions of events in the nearby Universe are assumed to correlate with sources in the 2MASS Redshift Survey (2MRS), IRAS 1.2 Jy Survey, Palermo Swift-BAT and Swift-BAT catalogs, and the effect of the latitude of the observatory on the measurement of the energy spectrum and on the capability of measuring anisotropy is studied. The differences between given latitudes on the northern and southern hemispheres are quantified. It is shown that the latitude of the observatory: a) has an influence on the total flux measured and b) imposes an important limitation on the capability of measuring an anisotropic sky.

  11. Microstructure of ultra high performance concrete containing lithium slag.

    Science.gov (United States)

    He, Zhi-Hai; Du, Shi-Gui; Chen, Deng

    2018-04-03

    Lithium slag (LS) is discharged as a byproduct in the process of the lithium carbonate, and it is very urgent to explore an efficient way to recycle LS in order to protect the environments and save resources. Many available supplementary cementitious materials for partial replacement of cement and/or silica fume (SF) can be used to prepare ultra high performance concrete (UHPC). The effect of LS to replace SF partially by weight used as a supplementary cementitious material (0%, 5%, 10% and 15% of binder) on the compressive strengths and microstructure evolution of UHPC has experimentally been studied by multi-techniques including mercury intrusion porosimetry, scanning electron microscope and nanoindentation technique. The results show that the use of LS degrades the microstructure of UHPC at early ages, and however, the use of LS with the appropriate content improves microstructure of UHPC at later ages. The hydration products of UHPC are mainly dominated by ultra-high density calcium-silicate-hydrate (UHD C-S-H) and interfacial transition zone (ITZ) in UHPC has similar compact microstructure with the matrix. The use of LS improves the hydration degree of UHPC and increases the elastic modulus of ITZ in UHPC. LS is a promising substitute for SF for preparation UHPC. Copyright © 2018 Elsevier B.V. All rights reserved.

  12. Systematic Calibration for Ultra-High Accuracy Inertial Measurement Units

    Directory of Open Access Journals (Sweden)

    Qingzhong Cai

    2016-06-01

    Full Text Available An inertial navigation system (INS has been widely used in challenging GPS environments. With the rapid development of modern physics, an atomic gyroscope will come into use in the near future with a predicted accuracy of 5 × 10−6°/h or better. However, existing calibration methods and devices can not satisfy the accuracy requirements of future ultra-high accuracy inertial sensors. In this paper, an improved calibration model is established by introducing gyro g-sensitivity errors, accelerometer cross-coupling errors and lever arm errors. A systematic calibration method is proposed based on a 51-state Kalman filter and smoother. Simulation results show that the proposed calibration method can realize the estimation of all the parameters using a common dual-axis turntable. Laboratory and sailing tests prove that the position accuracy in a five-day inertial navigation can be improved about 8% by the proposed calibration method. The accuracy can be improved at least 20% when the position accuracy of the atomic gyro INS can reach a level of 0.1 nautical miles/5 d. Compared with the existing calibration methods, the proposed method, with more error sources and high order small error parameters calibrated for ultra-high accuracy inertial measurement units (IMUs using common turntables, has a great application potential in future atomic gyro INSs.

  13. Live Ultra-High Definition from the International Space Station

    Science.gov (United States)

    Grubbs, Rodney; George, Sandy

    2017-01-01

    The first ever live downlink of Ultra-High Definition (UHD) video from the International Space Station (ISS) was the highlight of a 'Super Session' at the National Association of Broadcasters (NAB) in April 2017. The Ultra-High Definition video downlink from the ISS all the way to the Las Vegas Convention Center required considerable planning, pushed the limits of conventional video distribution from a space-craft, and was the first use of High Efficiency Video Coding (HEVC) from a space-craft. The live event at NAB will serve as a pathfinder for more routine downlinks of UHD as well as use of HEVC for conventional HD downlinks to save bandwidth. HEVC may also enable live Virtual Reality video downlinks from the ISS. This paper will describe the overall work flow and routing of the UHD video, how audio was synchronized even though the video and audio were received many seconds apart from each other, and how the demonstration paves the way for not only more efficient video distribution from the ISS, but also serves as a pathfinder for more complex video distribution from deep space. The paper will also describe how a 'live' event was staged when the UHD coming from the ISS had a latency of 10+ seconds. Finally, the paper will discuss how NASA is leveraging commercial technologies for use on-orbit vs. creating technology as was required during the Apollo Moon Program and early space age.

  14. Ultra-high pressure water jet: Baseline report

    International Nuclear Information System (INIS)

    1997-01-01

    The ultra-high pressure waterjet technology was being evaluated at Florida International University (FIU) as a baseline technology. In conjunction with FIU's evaluation of efficiency and cost, this report covers the evaluation conducted for safety and health issues. It is a commercially available technology and has been used for various projects at locations throughout the country. The ultra-high pressure waterjet technology acts as a cutting tool for the removal of surface substrates. The Husky trademark pump feeds water to a lance that directs the high pressure water at the surface to be removed. The safety and health evaluation during the testing demonstration focused on two main areas of exposure. These were dust and noise. The dust exposure was found to be minimal, which would be expected due to the wet environment inherent in the technology, but noise exposure was at a significant level. Further testing for noise is recommended because of the outdoor environment where the testing demonstration took place. In addition, other areas of concern found were arm-hand vibration, ergonomics, heat stress, tripping hazards, electrical hazards, lockout/tagout, fall hazards, slipping hazards, hazards associated with the high pressure water, and hazards associated with air pressure systems

  15. Magnetic resonance imaging and spectroscopy at ultra high fields

    International Nuclear Information System (INIS)

    Neuberger, Thomas

    2009-01-01

    The goal of the work presented in this thesis was to explore the possibilities and limitations of MRI / MRS using an ultra high field of 17.6 tesla. A broad range of specific applications and MR methods, from MRI to MRSI and MRS were investigated. The main foci were on sodium magnetic resonance spectroscopic imaging of rodents, magnetic resonance spectroscopy of the mouse brain, and the detection of small amounts of iron labeled stem cells in the rat brain using MRI Sodium spectroscopic imaging was explored since it benefits tremendously from the high magnetic field. Due to the intrinsically low signal in vivo, originating from the low concentrations and short transverse relaxation times, only limited results have been achieved by other researchers until now. Results in the literature include studies conducted on large animals such as dogs to animals as small as rats. No studies performed on mice have been reported, despite the fact that the mouse is the most important laboratory animal due to the ready availability of transgenic strains. Hence, this study concentrated on sodium MRSI of small rodents, mostly mice (brain, heart, and kidney), and in the case of the brain on young rats. The second part of this work concentrated on proton magnetic resonance spectroscopy of the rodent brain. Due to the high magnetic field strength not only the increasing signal but also the extended spectral resolution was advantageous for such kind of studies. The difficulties/limitations of ultra high field MRS were also investigated. In the last part of the presented work detection limits of iron labeled stem cells in vivo using magnetic resonance imaging were explored. The studies provided very useful benchmarks for future researchers in terms of the number of labeled stem cells that are required for high-field MRI studies. Overall this work has shown many of the benefits and the areas that need special attention of ultra high fields in MR. Three topics in MRI, MRS and MRSI were

  16. Magnetic resonance imaging and spectroscopy at ultra high fields

    Energy Technology Data Exchange (ETDEWEB)

    Neuberger, Thomas

    2009-06-23

    The goal of the work presented in this thesis was to explore the possibilities and limitations of MRI / MRS using an ultra high field of 17.6 tesla. A broad range of specific applications and MR methods, from MRI to MRSI and MRS were investigated. The main foci were on sodium magnetic resonance spectroscopic imaging of rodents, magnetic resonance spectroscopy of the mouse brain, and the detection of small amounts of iron labeled stem cells in the rat brain using MRI Sodium spectroscopic imaging was explored since it benefits tremendously from the high magnetic field. Due to the intrinsically low signal in vivo, originating from the low concentrations and short transverse relaxation times, only limited results have been achieved by other researchers until now. Results in the literature include studies conducted on large animals such as dogs to animals as small as rats. No studies performed on mice have been reported, despite the fact that the mouse is the most important laboratory animal due to the ready availability of transgenic strains. Hence, this study concentrated on sodium MRSI of small rodents, mostly mice (brain, heart, and kidney), and in the case of the brain on young rats. The second part of this work concentrated on proton magnetic resonance spectroscopy of the rodent brain. Due to the high magnetic field strength not only the increasing signal but also the extended spectral resolution was advantageous for such kind of studies. The difficulties/limitations of ultra high field MRS were also investigated. In the last part of the presented work detection limits of iron labeled stem cells in vivo using magnetic resonance imaging were explored. The studies provided very useful benchmarks for future researchers in terms of the number of labeled stem cells that are required for high-field MRI studies. Overall this work has shown many of the benefits and the areas that need special attention of ultra high fields in MR. Three topics in MRI, MRS and MRSI were

  17. Chiral chromatography-tandem mass spectrometry applied to the determination of pro-resolving lipid mediators.

    Science.gov (United States)

    Homann, Julia; Lehmann, Christoph; Kahnt, Astrid S; Steinhilber, Dieter; Parnham, Michael J; Geisslinger, Gerd; Ferreirós, Nerea

    2014-09-19

    Pro-resolving lipid mediators are a class of endogenously synthesized molecules derived from different fatty acids, such as arachidonic, docosahexaenoic or eicosapentaenoic acid, which are derived into four different product families: lipoxins, resolvins, maresins and protectins. For quantitation of these compounds, a sensitive, selective and robust liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous quantitation of lipoxin A4, 6-epi-lipoxin A4, lipoxin B4 and lipoxin A5, the D-series resolvins D1 and D2 as well as aspirin-triggered lipoxin A4 and resolvin D1, maresin and protectin and the pathway markers 17(S)-hydroxy-docosahexaenoic acid and 17(R)-hydroxy-docosahexaenoic acid in cell culture supernatants. For this purpose, a chiral column was connected in series with a reversed-phase column to achieve efficient analyte separation and high sensitivity. Sample pre-treatment included a fast and simple liquid-liquid extraction procedure. Limits of quantitation in the range of 0.1-0.5ng/mL cell culture media, absolute recoveries between 90 and 115%, intra- and interday precision of less than 13% and an accuracy of less than 11% were obtained. Stability of the samples after 60 days storage at -80°C, three freeze/thaw cycles and 4h at room temperature has been demonstrated for all analytes. Sample extracts can be stored at 7°C for 24h without degradation of the analytes. Deviations of less than 13% in the accuracy, evaluated in terms of relative error, were obtained. The suitability of the method has been demonstrated in cell culture supernatants of human polymorphonuclear leukocytes, stimulated with 15R-hydroxy-eicosatetraenoic acid and in cell culture media of human polymorphonuclear leukocytes co-incubated with human platelets. From all studied analytes, lipoxin A4 and 6-epi-lipoxin A4 were found in cell culture media under both incubation conditions, while 15-epi-lipoxin A4 was additionally detected in cell

  18. Comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones.

    Science.gov (United States)

    Carnes, Stephanie; O'Brien, Stacey; Szewczak, Angelica; Tremeau-Cayel, Lauriane; Rowe, Walter F; McCord, Bruce; Lurie, Ira S

    2017-09-01

    A comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones has been conducted. Nine different mixtures of bath salts were analyzed in this study. The three different chromatographic techniques were examined using a general set of controlled synthetic cathinones as well as a variety of other synthetic cathinones that exist as positional isomers. Overall 35 different synthetic cathinones were analyzed. A variety of column types and chromatographic modes were examined for developing each separation. For the ultra high performance supercritical fluid chromatography separations, analyses were performed using a series of Torus and Trefoil columns with either ammonium formate or ammonium hydroxide as additives, and methanol, ethanol or isopropanol organic solvents as modifiers. Ultra high performance liquid chromatographic separations were performed in both reversed phase and hydrophilic interaction chromatographic modes using SPP C18 and SPP HILIC columns. Gas chromatography separations were performed using an Elite-5MS capillary column. The orthogonality of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography was examined using principal component analysis. For the best overall separation of synthetic cathinones, the use of ultra high performance supercritical fluid chromatography in combination with gas chromatography is recommended. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Ultra-high current density thin-film Si diode

    Science.gov (United States)

    Wang, Qi [Littleton, CO

    2008-04-22

    A combination of a thin-film .mu.c-Si and a-Si:H containing diode structure characterized by an ultra-high current density that exceeds 1000 A/cm.sup.2, comprising: a substrate; a bottom metal layer disposed on the substrate; an n-layer of .mu.c-Si deposited the bottom metal layer; an i-layer of .mu.c-Si deposited on the n-layer; a buffer layer of a-Si:H deposited on the i-layer, a p-layer of .mu.c-Si deposited on the buffer layer; and a top metal layer deposited on the p-layer.

  20. Achieving Mixtures of Ultra-High Performance Concrete

    Directory of Open Access Journals (Sweden)

    Mircea POPA

    2013-07-01

    Full Text Available Ultra-High Performance Concrete (UHPC is a relatively new concrete. According to [11] UHPC is that concrete which features compressive strength over C100/115 class. Up to this point standards for this type of concrete were not adopted, although its characteristic strength exceeds those specified in [33]. Its main property is high compressive strength. This provides the possibility of reducing the section of elements (beams or columns made of this type of concrete, while the load capacity remains high. The study consists in blending mixtures of UHPC made of varying proportions of materials. The authors have obtained strengths of up to 160 MPa. The materials used are: Portland cement, silica fume, quartz powder, steel fibers, superplasticiser, sand and crushed aggregate for concrete - andesite.

  1. Evaluation of ISABELLE full cell ultra high vacuum system

    International Nuclear Information System (INIS)

    Foerster, C.L.; Briggs, J.; Chou, T.S.; Stattel, P.

    1980-01-01

    The ISABELLE Full Cell Vacuum System consisting of a 40 m long, by 8.8 cm diameter stainless steel tube pumped by seven pumping stations was assembled and processed for 10 -12 Torr operation. Evaluation and testing of the system and its sub-assemblies has been completed. Detail design of system components and the determination of the conditioning process was completed. The best procedure to rough pump, leak test, vacuum bake the system, condition pumps, degas gauges, turn on ion pumps and flash sublimation pumps was established. Pressures below 2 x 10 -11 Torr are now routinely achieved in normal operation of the Full Cell. This includes pump down after replacement of various components and pump down after back fill with moist unfiltered air. The techniques developed for the Full Cell will be used to build the ISABELLE Ultra High Vacuum System

  2. Ultra-high-ohmic microstripline resistors for Coulomb blockade devices

    International Nuclear Information System (INIS)

    Lotkhov, Sergey V

    2013-01-01

    In this paper, we report on the fabrication and low-temperature characterization of ultra-high-ohmic microstripline resistors made of a thin film of weakly oxidized titanium. Nearly linear voltage–current characteristics were measured at temperatures down to T ∼ 20 mK for films with sheet resistivities as high as ∼7 kΩ, i.e. about an order of magnitude higher than our previous findings for weakly oxidized Cr. Our analysis indicates that such an improvement can help to create an advantageous high-impedance environment for different Coulomb blockade devices. Further properties of the Ti film addressed in this work show the promise of low-noise behavior of the resistors when applied in different realizations of the quantum standard of current. (paper)

  3. Micro-damage propagation in ultra-high vacuum seals

    CERN Document Server

    Lutkiewicz, P; Garion, C

    2010-01-01

    The paper addresses a fundamental problem of tightness of ultra-high vacuum systems (UHV) at cryogenic temperatures in the light of continuum damage mechanics (CDM). The problem of indentation of a rigid punch into an elastic-plastic half-space is investigated based on rate independent plasticity with mixed kinematic and isotropic hardening. The micro-damage fields are modeled by using an anisotropic approach with a kinetic law of damage evolution suitable for ductile materials and cryogenic temperatures. The model has been experimentally validated and the results are used to predict the onset of macro-cracking (loss of tightness) and the corresponding load (contact pressure). The algorithm is applied in the design of UHV systems for particle accelerators. (C) 2009 Published by Elsevier Ltd.

  4. Ultra high energy electrons powered by pulsar rotation.

    Science.gov (United States)

    Mahajan, Swadesh; Machabeli, George; Osmanov, Zaza; Chkheidze, Nino

    2013-01-01

    A new mechanism of particle acceleration, driven by the rotational slow down of the Crab pulsar, is explored. The rotation, through the time dependent centrifugal force, can efficiently excite unstable Langmuir waves in the electron-positron (hereafter e(±)) plasma of the star magnetosphere. These waves, then, Landau damp on electrons accelerating them in the process. The net transfer of energy is optimal when the wave growth and the Landau damping times are comparable and are both very short compared to the star rotation time. We show, by detailed calculations, that these are precisely the conditions for the parameters of the Crab pulsar. This highly efficient route for energy transfer allows the electrons in the primary beam to be catapulted to multiple TeV (~ 100 TeV) and even PeV energy domain. It is expected that the proposed mechanism may, unravel the puzzle of the origin of ultra high energy cosmic ray electrons.

  5. Cosmic-ray ultra high-energy multijet family event

    International Nuclear Information System (INIS)

    Zou Bao-tang; Wang Cheng-rui; Ren Jing-ru

    1987-01-01

    A cosmic-ray ultra-high-energy multijet family event with visible energy of about 1500 TeV and five large cores is reported. This event was found in the 1980-1981 exposure of the Mt. Kambala (5500 M a.s.l.) emulsion-chamber experiment. The family characteristics are analyzed and compared with other cosmic ray events in the same energy range. The production and fragmentation characteristics of the five jets are studied and compared with the experimental results of accelerators and emulsion chamber C-jets as well as with QCD predictions above the TeV range. Some features on hadronic interactions in the TeV range are discussed

  6. Ultra-high-speed inversion recovery echo planar MR imaging

    International Nuclear Information System (INIS)

    Stehling, M.K.; Ordidge, R.J.; Coxon, R.; Chapman, B.; Houseman, A.M.; Guifoyle, D.; Blamire, A.; Gibbs, P.; Mansfield, P.

    1988-01-01

    Fast two-dimensional FT MR imaging techniques such as fast low-angle shot do not allow inversion recovery (IR). Rapid repetition of low-angle pulses is incompatible with a 180 0 inversion pulse. Echo planar imaging (EPI) can be applied in conjunction with IR, because after preparation of the spin system, a complete image is acquired. Data acquisition in less than 100 msec and real-time display allows interactive optimization of inversion time (4.0-9,000 msec) with little time penalty. The authors have applied IR EPI to the study of the brain, liver, and kidneys in normal volunteers and patients. Technical details are presented, and the applications of this first ultra-high-speed IR technique will be shown

  7. A mass census of the nearby universe with the RESOLVE survey

    Science.gov (United States)

    Eckert, Kathleen

    The galaxy mass function, i.e., the distribution of galaxies as a function of mass, is a useful way to characterize the galaxy population. In this work, we examine the stellar and baryonic mass function, and the velocity function of galaxies and galaxy groups for two volume-limited surveys of the nearby universe. Stellar masses are estimated from multi-band photometry, and we add cold atomic gas from measurements and a newly calibrated estimator to obtain baryonic mass. Velocities are measured from the internal motions of galaxies and groups and account for all matter within the system. We compare our observed mass and velocity functions with the halo mass function from theoretical simulations of dark matter, which predict a much more steeply rising low-mass slope than is normally observed for the galaxy mass function. We show that taking into account the cold gas mass, which dominates the directly detectable mass of low-mass galaxies, steepens the low-mass slope of the galaxy mass function. The low- mass slope of the baryonic mass function, however, is still much shallower than that of the halo mass function. The discrepancy in low-mass slope persists when examining the velocity function, which accounts for all matter in galaxies (detectable or not), suggesting that some mechanism must reduce the mass in halos or destroy them completely. We investigate the role of environment by performing group finding and examining the mass and velocity functions as a function of group halo mass. Broken down by halo mass regime, we find dips and varying low-mass slopes in the mass and velocity functions, suggesting that group formation processes such as merging and stripping, which destroy and lower the mass of low-mass satellites respectively, potentially contribute to the discrepancy in low-mass slope. In particular, we focus on the nascent group regime, groups of mass 10 11.4-12 [solar mass] with few members, which has a depressed and flat low-mass slope in the galaxy mass

  8. Towards a more common use of Ultra-High Performance Concrete (UHPC) – development of UHPC for ready-mix and prefabrication concrete plants

    NARCIS (Netherlands)

    Spiesz, P.R.; Hunger, M.; Justnes, Harald; Braarud, Henny

    2017-01-01

    This study addresses the development of ultra-high performance concrete (UHPC) suitable for a mass production in conventional ready-mix and prefabrication concrete plants. In order to facilitate the production process, curing regime and to minimize the costs, no additional treatments (e.g. thermal

  9. Characterization and usage of the EASY-spray technology as part of an online 2D SCX-RP ultra-high pressure system

    NARCIS (Netherlands)

    Marino, Fabio; Cristobal, Alba; Binai, Nadine A; Bache, Nicolai; Heck, Albert J R; Mohammed, Shabaz

    2014-01-01

    Ultra-high pressure liquid chromatography (UHPLC) systems combined with state-of-the-art mass spectrometers have pushed the limit of deep proteome sequencing to new heights making it possible to identify thousands of proteins in a single LC-MS experiment within a few hours. The recently released

  10. A useful PET probe [11C]BU99008 with ultra-high specific radioactivity for small animal PET imaging of I2-imidazoline receptors in the hypothalamus

    International Nuclear Information System (INIS)

    Kawamura, Kazunori; Shimoda, Yoko; Yui, Joji; Zhang, Yiding; Yamasaki, Tomoteru; Wakizaka, Hidekatsu; Hatori, Akiko; Xie, Lin; Kumata, Katsushi; Fujinaga, Masayuki; Ogawa, Masanao; Kurihara, Yusuke; Nengaki, Nobuki; Zhang, Ming-Rong

    2017-01-01

    Introduction: A positron emission tomography (PET) probe with ultra-high specific radioactivity (SA) enables measuring high receptor specific binding in brain regions by avoiding mass effect of the PET probe itself. It has been reported that PET probe with ultra-high SA can detect small change caused by endogenous or exogenous ligand. Recently, Kealey et al. developed [ 11 C]BU99008, a more potent PET probe for I 2 -imidazoline receptors (I 2 Rs) imaging, with a conventional SA (mean 76 GBq/μmol) showed higher specific binding in the brain. Here, to detect small change of specific binding for I 2 Rs caused by endogenous or exogenous ligand in an extremely small region, such as hypothalamus in the brain, we synthesized and evaluated [ 11 C]BU99008 with ultra-high SA as a useful PET probe for small-animal PET imaging of I 2 Rs. Methods: [ 11 C]BU99008 was prepared by [ 11 C]methylation of N-desmethyl precursor with [ 11 C]methyl iodide. Biodistribution, metabolite analysis, and brain PET studies were conducted in rats. Results: [ 11 C]BU99008 with ultra-high SA in the range of 5400–16,600 GBq/μmol were successfully synthesized (n = 7), and had appropriate radioactivity for in vivo study. In the biodistribution study, the mean radioactivity levels in all investigated tissues except for the kidney did not show significant difference between [ 11 C]BU99008 with ultra-high SA and that with conventional SA. In the metabolite analysis, the percentage of unchanged [ 11 C]BU99008 at 30 min after the injection of probes with ultra-high and conventional SA was similar in rat brain and plasma. In the PET study of rats' brain, radioactivity level (AUC 30–60 min ) in the hypothalamus of rats injected with [ 11 C]BU99008 with ultra-high SA (64 [SUV ∙ min]) was significantly higher than that observed for that with conventional SA (50 [SUV ∙ min]). The specific binding of [ 11 C]BU99008 with ultra-high SA (86% of total binding) for I 2 R was higher than that of

  11. An Evaluation of Ultra-High Pressure Regulator for Robotic Lunar Landing Spacecraft

    Science.gov (United States)

    Burnside, Christopher; Trinh, Huu; Pedersen, Kevin

    2011-01-01

    The Robotic Lunar Lander Development (RLLD) Project Office at NASA Marshall Space Flight Center (MSFC) has studied several lunar surface science mission concepts. These missions focus on spacecraft carrying multiple science instruments and power systems that will allow extended operations on the lunar surface. Initial trade studies of launch vehicle options for these mission concepts indicate that the spacecraft design will be significantly mass-constrained. To minimize mass and facilitate efficient packaging, the notional propulsion system for these landers has a baseline of an ultra-high pressure (10,000 psig) helium pressurization system that has been used on Defense missiles. The qualified regulator is capable of short duration use; however, the hardware has not been previously tested at NASA spacecraft requirements with longer duration. Hence, technical risks exist in using this missile-based propulsion component for spacecraft applications. A 10,000-psig helium pressure regulator test activity is being carried out as part of risk reduction testing for MSFC RLLD project. The goal of the test activity is to assess the feasibility of commercial off-the-shelf ultra-high pressure regulator by testing with a representative flight mission profile. Slam-start, gas blowdown, water expulsion, lock-up, and leak tests are also performed on the regulator to assess performance under various operating conditions. The preliminary test results indicated that the regulator can regulate helium to a stable outlet pressure of 740 psig within the +/- 5% tolerance band and maintain a lock-up pressure less than +5% for all tests conducted. Numerous leak tests demonstrated leakage less than 10-3 standard cubic centimeters per second (SCCS) for internal seat leakage at lock-up and less than10-5 SCCS for external leakage through the regulator ambient reference cavity. The successful tests have shown the potential for 10,000 psig helium systems in NASA spacecraft and have reduced risk

  12. Design and performance of a soft-x-ray interferometer for ultra-high-resolution fourier transform spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Moler, E.J.; Hussain, Z.; Duarte, R.M.; Howells, M.R. [Lawrence Berkeley National Lab., CA (United States)

    1997-04-01

    A Fourier Transform Soft X-ray spectrometer (FT-SX) has been designed and is under construction for the Advanced Light Source (ALS) at Lawrence Berkeley National Laboratory as a branch of beamline 9.3.2. The spectrometer is a novel soft x-ray interferometer designed for ultra-high resolution (theoretical resolving power E/{delta}E{approximately}10{sup 6}) spectroscopy in the photon energy region of 60-120 eV. This instrument is expected to provide experimental results which sensitively test models of correlated electron processes in atomic and molecular physics. The design criteria and consequent technical challenges posed by the short wavelengths of x-rays and desired resolving power are discussed. The fundamental and practical aspects of soft x-ray interferometry are also explored.

  13. Generation, insulated confinement, and heating of ultra-high temperature plasmas

    International Nuclear Information System (INIS)

    Bass, R.W.

    1986-01-01

    This invention relates to the production and maintenance in steady state of ultra-high temperature confined plasmas, particularly those created by full ionization of a volume of some hydrogenic gas such as deuterium. The target mass is surrounded with an ambient fluid medium at a predetermined pressure. Pulsed energy is projected upon the target mass to bring it to a predetermined temperature and to fully ionize it; this energy may be pulsed photon energy or pulsed particle-beam kinetic energy. An electrostatic double layer is formed spontaneously between the ionized mass and the ambient medium, providing thermal insulation and leaving the dominant energy loss to be bremmstrahlung losses. The bremmstrahlung losses are compensated for completely by supplying additional radiant energy to the ionized mass to maintain its temperature. The frequency range of the additional radiant energy is selected so as to be absorbable by the ionized mass, and its power level is adjusted to maintain the ionized mass in a substantially steady state. The static pressure of the ambient medium is increased, thereby equally increasing the static pressure of the ionized mass so as to enable the mass to absorb more of the radiant energy and increasing its temperature but also increasing its power losses. Simultaneously the radius and temperature of the mass are monitored and the power level of the radiant energy supply is increased to as to compensate for the power losses. The minimum feasible size of the plasma is less than a centimeter in diameter, while there is no constraint on maximum feasible size. This invention may be practiced with commercially-available lasers and microwave beam generators

  14. 75 FR 81284 - Nationwide Use of High Frequency and Ultra High Frequency Active SONAR Technology; Draft...

    Science.gov (United States)

    2010-12-27

    ... Frequency and Ultra High Frequency Active SONAR Technology; Draft Programmatic Environmental Assessment and... Programmatic Environmental Assessment (PEA) for the Nationwide Use of High Frequency (HF) and Ultra High... potential impacts of each alternative on the human and natural environments. DATES: Comments and related...

  15. Ultra high performance concrete made with rice husk ash for reduced autogenous shrinkage

    NARCIS (Netherlands)

    Van Breugel, K.; Van Tuan, N.

    2014-01-01

    Ultra High Strength Concrete (UHPC) is generally made with low w/c mixtures and by adding silica fume. Low w/c mixtures, however, exhibit high autogenous shrinkage, while a high amount of silica fume increases the price of these mixtures. For designing ultra high strength mixtures with low

  16. Ultra-high field MRI: Advancing systems neuroscience towards mesoscopic human brain function

    NARCIS (Netherlands)

    Dumoulin, Serge O; Fracasso, A.; Van der Zwaag, W.; Siero, Jeroen C W; Petridou, Natalia

    2018-01-01

    Human MRI scanners at ultra-high magnetic field strengths of 7 T and higher are increasingly available to the neuroscience community. A key advantage brought by ultra-high field MRI is the possibility to increase the spatial resolution at which data is acquired, with little reduction in image

  17. MHD Modeling of Conductors at Ultra-High Current Density

    International Nuclear Information System (INIS)

    ROSENTHAL, STEPHEN E.; DESJARLAIS, MICHAEL P.; SPIELMAN, RICK B.; STYGAR, WILLIAM A.; ASAY, JAMES R.; DOUGLAS, M.R.; HALL, C.A.; FRESE, M.H.; MORSE, R.L.; REISMAN, D.B.

    2000-01-01

    In conjunction with ongoing high-current experiments on Sandia National Laboratories' Z accelerator, the authors have revisited a problem first described in detail by Heinz Knoepfel. Unlike the 1-Tesla MITLs of pulsed power accelerators used to produce intense particle beams, Z's disc transmission line (downstream of the current addition) is in a 100--1,200 Tesla regime, so its conductors cannot be modeled simply as static infinite conductivity boundaries. Using the MHD code MACH2 they have been investigating the conductor hydrodynamics, characterizing the joule heating, magnetic field diffusion, and material deformation, pressure, and velocity over a range of current densities, current rise-times, and conductor materials. Three purposes of this work are (1) to quantify power flow losses owing to ultra-high magnetic fields, (2) to model the response of VISAR diagnostic samples in various configurations on Z, and (3) to incorporate the most appropriate equation of state and conductivity models into the MHD computations. Certain features are strongly dependent on the details of the conductivity model

  18. Application of ultra high pressure (UHP) in starch chemistry.

    Science.gov (United States)

    Kim, Hyun-Seok; Kim, Byung-Yong; Baik, Moo-Yeol

    2012-01-01

    Ultra high pressure (UHP) processing is an attractive non-thermal technique for food treatment and preservation at room temperature, with the potential to achieve interesting functional effects. The majority of UHP process applications in food systems have focused on shelf-life extension associated with non-thermal sterilization and a reduction or increase in enzymatic activity. Only a few studies have investigated modifications of structural characteristics and/or protein functionalities. Despite the rapid expansion of UHP applications in food systems, limited information is available on the effects of UHP on the structural and physicochemical properties of starch and/or its chemical derivatives included in most processed foods as major ingredients or minor additives. Starch and its chemical derivatives are responsible for textural and physical properties of food systems, impacting their end-use quality and/or shelf-life. This article reviews UHP processes for native (unmodified) starch granules and their effects on the physicochemical properties of UHP-treated starch. Furthermore, functional roles of UHP in acid-hydrolysis, hydroxypropylation, acetylation, and cross-linking reactions of starch granules, as well as the physicochemical properties of UHP-assisted starch chemical derivatives, are discussed.

  19. Fracture toughness of ultra high performance concrete by flexural performance

    Directory of Open Access Journals (Sweden)

    Manolova Emanuela

    2016-01-01

    Full Text Available This paper describes the fracture toughness of the innovative structural material - Ultra High Performance Concrete (UHPC, evaluated by flexural performance. For determination the material behaviour by static loading are used adapted standard test methods for flexural performance of fiber-reinforced concrete (ASTM C 1609 and ASTM C 1018. Fracture toughness is estimated by various deformation parameters derived from the load-deflection curve, obtained by testing simple supported beam under third-point loading, using servo-controlled testing system. This method is used to be estimated the contribution of the embedded fiber-reinforcement into improvement of the fractural behaviour of UHPC by changing the crack-resistant capacity, fracture toughness and energy absorption capacity with various mechanisms. The position of the first crack has been formulated based on P-δ (load- deflection response and P-ε (load - longitudinal deformation in the tensile zone response, which are used for calculation of the two toughness indices I5 and I10. The combination of steel fibres with different dimensions leads to a composite, having at the same time increased crack resistance, first crack formation, ductility and post-peak residual strength.

  20. Some aspects of ultra high energy gamma ray astronomy

    International Nuclear Information System (INIS)

    De Jager, O.C.

    1983-11-01

    A short review of ultra high energy (UHE) gamma ray astronomy (10 11 14 eV) as well as a description of a planned experiment to be erected at Potchefstroom is given in the introduction. This experiment will be the first and only one in the Southern Hemisphere and as such may play an important role in this new field of astronomy and astrophysics. In the first part the necessary infrastructure for astronomical observations of known celestial objects is developed. This embodies the special physical, mechanical and astronomical constraints in this type of astronomy, such as the definition of the various astronomical coordinate systems and transformations between them, the effect of precession and nutation on the source position etc. This leads to automatic observation schedules for the various applicable techniques of observation. In the second part the various effects which may influence the arrival time of a gamma ray at the telescope is investigated. It is found that dispersion and relativistic effects are negligible, given the special type of analysis used in this low counting rate system. The classic Doppler effect due to the motion of Earth as well as the configuration of the telescope does have a major effect and must be taken into consideration when analysing the data. A simple method, depending only on the movement of Earth around the sun, is developed to simplify the identification of pulsars at the planned observatory where computing facilities are limited

  1. A new generation of ultra high strength steel pipelines

    International Nuclear Information System (INIS)

    Brozda, J.; Zeman, M.; Weglowski, M.

    2008-01-01

    For many years an increased demand for natural gas can be observed. Ultra high-strength pipelines with higher operating pressures and/or reduced wall thickness are a means to reduce transmission costs. Motivated by reduced investment costs (overcharge a few billion of dollars), tend towards the development of a new grade of pipeline steel with microalloying element for example Nb, that potentially lowers the total cost of long-distance gas pipelines by 5 - 15%. New long distance pipelines have budgets in excess of several billion dollars. This paper describes mechanical properties of new generation of pipelines steel with higher content of niobium and the influence the welding thermal cycles on the microstructure and brittle fracture resistance. The resistance to cold cracking has also been determined. It was found that the new steel has close properties to API X70 grade steels, but is cheaper in manufacturing and installation. The steel has been covered by the amended EN 10028-5 standard and proper modifications will also be made in other European standards. (author)

  2. SLC polarized beam source ultra-high-vacuum design

    International Nuclear Information System (INIS)

    Lavine, T.L.; Clendenin, J.E.; Garwin, E.L.; Hoyt, E.W.; Hoyt, M.W.; Miller, R.H.; Nuttall, J.A.; Schultz, D.C.; Wright, D.

    1991-05-01

    This paper describes the design of the ultra-high vacuum system for the beam-line from the 160-kV polarized electron gun to the linac injector in the Stanford Linear Collider (SLC). The polarized electron source is a GaAs photocathode, requiring 10 -11 -Torr-range pressure for adequate quantum efficiency and longevity. The photo-cathode is illuminated by 3-nsec-long laser pulses. Photo-cathode maintenance and improvements require occasional substitution of guns with rapid restoration of UHV conditions. Differential pumping is crucial since the pressure in the injector is more than 10 times greater than the photocathode can tolerate, and since electron-stimulated gas desorption from beam loss in excess of 0.1% of the 20-nC pulses may poison the photocathode. Our design for the transport line contains a differential pumping region isolated by a pair of valves. Exchange of guns requires venting only this isolated region which can be restored to UHV rapidly by baking. The differential pumping is performed by non-evaporable getters (NEGs) and an ion pump. 3 refs., 3 figs

  3. Fibrous Fillers to Manufacture Ultra High Ash/Performance Paper

    Energy Technology Data Exchange (ETDEWEB)

    Dr. VIjay K. Mathur

    2009-04-30

    The paper industry is one of the largest users of energy and emitters of CO2 in the US manufacturing industry. In addition to that, it is facing tremendous financial pressure due to lower cost imports. The fine paper industry has shrunk from 15 million tons per year production to 10 million tons per year in the last 5 years. This has resulted in mill closures and job loses. The AF&PA and the DOE formed a program called Agenda 2020 to help in funding to develop breakthrough technologies to provide help in meeting these challenges. The objectives of this project were to optimize and scale-up Fibrous Fillers technology, ready for commercial deployment and to develop ultra high ash/high performance paper using Fibrous Fillers. The goal was to reduce energy consumption, carbon footprint, and cost of manufacturing paper and related industries. GRI International (GRI) has been able to demonstrate the techno - economic feasibility and economic advantages of using its various products in both handsheets as well as in commercial paper mills. GRI has also been able to develop sophisticated models that demonstrate the effect of combinations of GRI's fillers at multiple filler levels. GRI has also been able to develop, optimize, and successfully scale-up new products for use in commercial paper mills.

  4. Evaluation of Ultra-High Temperature Ceramics for Aeropropulsion Use

    Science.gov (United States)

    Levine, Stanley R.; Opila, Elizabeth J.; Halbig, Michael C.; Kiser, James D.; Singh, Mrityunjay; Salem, Jonathan A.

    2001-01-01

    Among the ultra-high temperature ceramics (UHTC) are a group of materials consisting of zirconium diboride or hafnium diboride plus silicon carbide, and in some instances, carbon. These materials offer a good combination of properties that make them candidates for airframe leading edges on sharp-bodied reentry vehicles. These UHTC perform well in the environment for such applications, i.e., air at low pressure. The purpose of this study was to examine three of these materials under conditions more representative of a propulsion environment, i.e., higher oxygen partial pressure and total pressure. Results of strength and fracture toughness measurements, furnace oxidation and high velocity thermal shock exposures are presented for ZrB2 plus 20 volume % SiC, ZrB2 plus 14 volume % SiC plus 30 volume % C, and SCS-9a SiC fiber reinforced ZrB2 plus 20 volume % SiC. The poor oxidation resistance of UHTCs is the predominant factor limiting their applicability to propulsion applications.

  5. Ultra high resolution soft x-ray tomography

    International Nuclear Information System (INIS)

    Haddad, W.S.; Trebes, J.E.; Goodman, D.M.; Lee, H.R.; McNulty, I.; Zalensky, A.O.

    1995-01-01

    Ultra high resolution three dimensional images of a microscopic test object were made with soft x-rays using a scanning transmission x-ray microscope. The test object consisted of two different patterns of gold bars on silicon nitride windows that were separated by ∼5 microm. A series of nine 2-D images of the object were recorded at angles between -50 to +55 degrees with respect to the beam axis. The projections were then combined tomographically to form a 3-D image by means of an algebraic reconstruction technique (ART) algorithm. A transverse resolution of ∼ 1,000 angstrom was observed. Artifacts in the reconstruction limited the overall depth resolution to ∼ 6,000 angstrom, however some features were clearly reconstructed with a depth resolution of ∼ 1,000 angstrom. A specially modified ART algorithm and a constrained conjugate gradient (CCG) code were also developed as improvements over the standard ART algorithm. Both of these methods made significant improvements in the overall depth resolution, bringing it down to ∼ 1,200 angstrom overall. Preliminary projection data sets were also recorded with both dry and re-hydrated human sperm cells over a similar angular range

  6. Ultra high resolution soft x-ray tomography

    International Nuclear Information System (INIS)

    Haddad, W.S.; Trebes, J.E.; Goodman, D.M.

    1995-01-01

    Ultra high resolution three dimensional images of a microscopic test object were made with soft x-rays using a scanning transmission x-ray microscope. The test object consisted of two different patterns of gold bars on silicon nitride windows that were separated by ∼5μm. A series of nine 2-D images of the object were recorded at angles between -50 to +55 degrees with respect to the beam axis. The projections were then combined tomographically to form a 3-D image by means of an algebraic reconstruction technique (ART) algorithm. A transverse resolution of ∼1000 Angstrom was observed. Artifacts in the reconstruction limited the overall depth resolution to ∼6000 Angstrom, however some features were clearly reconstructed with a depth resolution of ∼1000 Angstrom. A specially modified ART algorithm and a constrained conjugate gradient (CCG) code were also developed as improvements over the standard ART algorithm. Both of these methods made significant improvements in the overall depth resolution bringing it down to ∼1200 Angstrom overall. Preliminary projection data sets were also recorded with both dry and re-hydrated human sperm cells over a similar angular range

  7. An ultra-high speed whole slide image viewing system.

    Science.gov (United States)

    Yagi, Yukako; Yoshioka, Shigeatsu; Kyusojin, Hiroshi; Onozato, Maristela; Mizutani, Yoichi; Osato, Kiyoshi; Yada, Hiroaki; Mark, Eugene J; Frosch, Matthew P; Louis, David N

    2012-01-01

    One of the goals for a Whole Slide Imaging (WSI) system is implementation in the clinical practice of pathology. One of the unresolved problems in accomplishing this goal is the speed of the entire process, i.e., from viewing the slides through making the final diagnosis. Most users are not satisfied with the correct viewing speeds of available systems. We have evaluated a new WSI viewing station and tool that focuses on speed. A prototype WSI viewer based on PlayStation®3 with wireless controllers was evaluated at the Department of Pathology at MGH for the following reasons: 1. For the simulation of signing-out cases; 2. Enabling discussion at a consensus conference; and 3. Use at slide seminars during a Continuing Medical Education course. Pathologists were being able to use the system comfortably after 0-15 min training. There were no complaints regarding speed. Most pathologists were satisfied with the functionality, usability and speed of the system. The most difficult situation was simulating diagnostic sign-out. The preliminary results of adapting the Sony PlayStation®3 (PS3®) as an ultra-high speed WSI viewing system were promising. The achieved speed is consistent with what would be needed to use WSI in daily practice.

  8. MHD Modeling of Conductors at Ultra-High Current Density

    International Nuclear Information System (INIS)

    Rosenthal, S.E.; Asay, J.R.; Desjarlais, M.P.; Douglas, M.R.; Frese, M.H.; Hall, C.A.; Morse, R.L.; Reisman, D.; Spielman, R.B.; Stygar, W.A.

    1999-01-01

    In conjunction with ongoing high-current experiments on Sandia National Laboratories' Z accelerator we have revisited a problem first described in detail by Heinz Knoepfel. MITLs of previous pulsed power accelerators have been in the 1-Tesla regime. Z's disc transmission line (downstream of the current addition) is in a 100-1200 Tesla regime, so its conductors cannot be modeled simply as static infinite conductivity boundaries. Using the MHD code MACH2 we have been investigating conductor hydrodynamics, characterizing the joule heating, magnetic field diffusion, and material deformation, pressure, and velocity over a range of current densities, current rise-times, and conductor materials. Three purposes of this work are ( 1) to quantify power flow losses owing to ultra-high magnetic fields, (2) to model the response of VISAR diagnostic samples in various configurations on Z, and (3) to incorporate the most appropriate equation of state and conductivity models into our MHD computations. Certain features are strongly dependent on the details of the conductivity model. Comparison with measurements on Z will be discussed

  9. Vacuum improvements for ultra high charge state ion acceleration

    International Nuclear Information System (INIS)

    Xie, Z.Q.; Lyneis, C.M.; Clark, D.J.; Guy, A.; Lundgren, S.A

    1998-06-01

    The installation of a second cryo panel has significantly improved the vacuum in the 88-Inch Cyclotron at Lawrence Berkeley National Laboratory. The neutral pressure in the extraction region decreased from 1.2 x 10 -6 down to about 7 x 10 -7 Torr. The vacuum improvement reduces beam loss from charge changing collisions and enhances the cyclotron beam transmission, especially for the high charge state heavy ions. Tests with improved vacuum show the cyclotron transmission increased more than 50% (from 5.7% to 9.0%) for a Xe 27+ at 603 MeV, more than doubled for a Bi 41+ beam (from 1.9% to 4.6%) at 904 MeV and tripled for a U 47+ beam (from 1.2% to 3.6%) at 1,115 MeV. At about 5 NeV/nucleon 92 enA (2.2 pnA) for Bi 41+ and 14 enA (0.3 pnA) for U 47+ were extracted ut of the 88-Inch Cyclotron Ion beams with charge states as high as U 64+ have been produced by the LBNL AECR-U ion source and accelerated through the cyclotron for the first time. The beam losses for a variety of ultra high charge state ions were measured as a function of cyclotron pressure and compared with the calculations from the existing models

  10. Vacuum improvements for ultra high charge state ion acceleration

    International Nuclear Information System (INIS)

    Xie, Z.Q.; Lyneis, C.M.; Clark, D.J.; Guy, A.; Lundgren, S.A.

    1999-01-01

    The installation of a second cryo panel has significantly improved the vacuum in the 88-Inch Cyclotron at Lawrence Berkeley National Laboratory. The neutral pressure in the extraction region decreased from 1.2 x 10 -6 down to about 7 x 10 -7 Torr. The vacuum improvement reduces beam loss from charge changing collisions and enhances the cyclotron beam transmission, especially for the high charge state heavy ions. Tests with improved vacuum show the cyclotron transmission increased more than 50% (from 5.7% to 9.0%) for a Xe 27+ at 603 MeV, more than doubled for a Bi 41+ beam (from 1.9% % to 4.6%) at 904 MeV and tripled for a U 47+ beam (from 1.2% to 3.6%) at 1115 MeV. At about 5 MeV/nucleon 92 enA (2.2 pnA) for Bi 41+ and 14 enA (0.3 pnA) for U 47+ were extracted out of the 88-Inch Cyclotron Ion beams with charge states as high as U 64+ have been produced by the LBNL AECR-U ion source and accelerated through the cyclotron for the first time. The beam losses for a variety of ultra high charge state ions were measured as a function of cyclotron pressure and compared with the calculations from the existing models. (authors)

  11. Ultra high frequency induction welding of powder metal compacts

    Directory of Open Access Journals (Sweden)

    Çavdar, Uǧur

    2014-06-01

    Full Text Available The application of the iron based Powder Metal (PM compacts in Ultra High Frequency Induction Welding (UHFIW were reviewed. These PM compacts are used to produce cogs. This study investigates the methods of joining PM materials enforceability with UHFIW in the industry application. Maximum stress and maximum strain of welded PM compacts were determined by three point bending and strength tests. Microhardness and microstructure of induction welded compacts were determined.Soldadura por inducción de ultra alta frecuencia de polvos de metal compactados. Se ha realizado un estudio de la aplicación de polvos de metal (PM de base hierro compactados por soldadura por inducción de ultra alta frecuencia (UHFIW. Estos polvos de metal compactados se utilizan para producir engranajes. Este estudio investiga los métodos de uni.n de los materiales de PM con UHFIW en su aplicación en la industria. La máxima tensión y la máxima deformación de los polvos de metal compactados soldados fueron determinadas por flexión en tres puntos y prueba de resistencia. Se determinó la microdureza y la microestructura de los polvos compactados por soldadura por inducción.

  12. Mass density slope of elliptical galaxies from strong lensing and resolved stellar kinematics

    Science.gov (United States)

    Lyskova, N.; Churazov, E.; Naab, T.

    2018-04-01

    We discuss constraints on the mass density distribution (parametrized as ρ ∝ r-γ) in early-type galaxies provided by strong lensing and stellar kinematics data. The constraints come from mass measurements at two `pinch' radii. One `pinch' radius r1 = 2.2REinst is defined such that the Einstein (i.e. aperture) mass can be converted into the spherical mass almost independently of the mass-model. Another `pinch' radius r2 = Ropt is chosen so that the dynamical mass, derived from the line-of-sight velocity dispersion, is least sensitive to the anisotropy of stellar orbits. We verified the performance of this approach on a sample of simulated elliptical galaxies and on a sample of 15 SLACS lens galaxies at 0.01 ≤ z ≤ 0.35, which have already been analysed in Barnabè et al. by the self-consistent joint lensing and kinematic code. For massive simulated galaxies, the density slope γ is recovered with an accuracy of ˜13 per cent, unless r1 and r2 happen to be close to each other. For SLACS galaxies, we found good overall agreement with the results of Barnabè et al. with a sample-averaged slope γ = 2.1 ± 0.05. Although the two-pinch-radii approach has larger statistical uncertainties, it is much simpler and uses only few arithmetic operations with directly observable quantities.

  13. Post-mortem inference of the human hippocampal connectivity and microstructure using ultra-high field diffusion MRI at 11.7 T.

    Science.gov (United States)

    Beaujoin, Justine; Palomero-Gallagher, Nicola; Boumezbeur, Fawzi; Axer, Markus; Bernard, Jeremy; Poupon, Fabrice; Schmitz, Daniel; Mangin, Jean-François; Poupon, Cyril

    2018-06-01

    The human hippocampus plays a key role in memory management and is one of the first structures affected by Alzheimer's disease. Ultra-high magnetic resonance imaging provides access to its inner structure in vivo. However, gradient limitations on clinical systems hinder access to its inner connectivity and microstructure. A major target of this paper is the demonstration of diffusion MRI potential, using ultra-high field (11.7 T) and strong gradients (750 mT/m), to reveal the extra- and intra-hippocampal connectivity in addition to its microstructure. To this purpose, a multiple-shell diffusion-weighted acquisition protocol was developed to reach an ultra-high spatio-angular resolution with a good signal-to-noise ratio. The MRI data set was analyzed using analytical Q-Ball Imaging, Diffusion Tensor Imaging (DTI), and Neurite Orientation Dispersion and Density Imaging models. High Angular Resolution Diffusion Imaging estimates allowed us to obtain an accurate tractography resolving more complex fiber architecture than DTI models, and subsequently provided a map of the cross-regional connectivity. The neurite density was akin to that found in the histological literature, revealing the three hippocampal layers. Moreover, a gradient of connectivity and neurite density was observed between the anterior and the posterior part of the hippocampus. These results demonstrate that ex vivo ultra-high field/ultra-high gradients diffusion-weighted MRI allows the mapping of the inner connectivity of the human hippocampus, its microstructure, and to accurately reconstruct elements of the polysynaptic intra-hippocampal pathway using fiber tractography techniques at very high spatial/angular resolutions.

  14. Native oxidation of ultra high purity Cu bulk and thin films

    International Nuclear Information System (INIS)

    Iijima, J.; Lim, J.-W.; Hong, S.-H.; Suzuki, S.; Mimura, K.; Isshiki, M.

    2006-01-01

    The effect of microstructure and purity on the native oxidation of Cu was studied by using angle-resolved X-ray photoelectron spectroscopy (AR-XPS) and spectroscopic ellipsometry (SE). A high quality copper film prepared by ion beam deposition under a substrate bias voltage of -50 V (IBD Cu film at V s = -50 V) showed an oxidation resistance as high as an ultra high purity copper (UHP Cu) bulk, whereas a Cu film deposited without substrate bias voltage (IBD Cu film at V s = 0 V) showed lower oxidation resistance. The growth of Cu 2 O layer on the UHP Cu bulk and both types of the films obeyed in principle a logarithmic rate law. However, the growth of oxide layer on the IBD Cu films at V s = 0 and -50 V deviated upward from the logarithmic rate law after the exposure time of 320 and 800 h, respectively. The deviation from the logarithmic law is due to the formation of CuO on the Cu 2 O layer after a critical time

  15. Size resolved mass concentration and elemental composition of atmospheric aerosols over the Eastern Mediterranean area

    Directory of Open Access Journals (Sweden)

    J. Smolík

    2003-01-01

    Full Text Available A Berner low pressure impactor was used to collect size-segregated aerosol samples at Finokalia, located on the north-eastern coast of Crete, Greece during July 2000 and January 2001. Several samples were also collected during the summer campaign aboard the research vessel "AEGAIEO" in the Aegean Sea. Gravimetric analysis and inversion techniques yielded daily PM1 and PM10 mass concentrations. The samples were also analysed by PIXE giving the elemental size distributions of Al, Si, K, Ca, Ti, Mn, Fe, Sr, S, Cl, Ni, V, Cu, Cr, Zn, and Pb. The crustal elements and sea-salt had a unimodal supermicron size distribution. Sulphur was found predominantly in submicron fractions. K, V, and Ni exhibited a bimodal distribution with a submicron mode produced by forest fires and oil combustion. The anthropogenic elements had broad and not well-defined distributions. The time series for PM1 and PM10 mass and elemental concentrations showed both daily and seasonal variation. Higher mass concentrations were observed during two incursions of Saharan dust, whilst higher concentrations of S, Cu, Zn, and Pb were encountered in samples collected in air masses arriving from northern Greece or the western coast of Turkey. Elevated concentrations of chlorine were found in samples with air masses either originating above the Atlantic Ocean and arriving at Finokalia via western Europe or recirculating over the western coast of the Black Sea.

  16. Characterization of Lipid A Variants by Energy-Resolved Mass Spectrometry: Impact of Acyl Chains

    Science.gov (United States)

    Crittenden, Christopher M.; Akin, Lucas D.; Morrison, Lindsay J.; Trent, M. Stephen; Brodbelt, Jennifer S.

    2017-06-01

    Lipid A molecules consist of a diglucosamine sugar core with a number of appended acyl chains that vary in their length and connectivity. Because of the challenging nature of characterizing these molecules and differentiating between isomeric species, an energy-resolved MS/MS strategy was undertaken to track the fragmentation trends and map genealogies of product ions originating from consecutive cleavages of acyl chains. Generalizations were developed based on the number and locations of the primary and secondary acyl chains as well as variations in preferential cleavages arising from the location of the phosphate groups. Secondary acyl chain cleavage occurs most readily for lipid A species at the 3' position, followed by primary acyl chain fragmentation at both the 3' and 3 positions. In the instances of bisphosphorylated lipid A variants, phosphate loss occurs readily in conjunction with the most favorable primary and secondary acyl chain cleavages. [Figure not available: see fulltext.

  17. Detection of seventy-two anabolic and androgenic steroids and/or their esters in horse hair using ultra-high performance liquid chromatography-high resolution mass spectrometry in multiplexed targeted MS2 mode and gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Choi, Timmy L S; Kwok, Karen Y; Kwok, Wai Him; Tsoi, Yeuki Y K; Wong, Jenny K Y; Wan, Terence S M

    2018-06-20

    Anabolic and androgenic steroids (AAS) are banned substances in both human and equine sports. They are often administered intramuscularly to horses in esterified forms for the purpose of extending their time of action. The authors' laboratory has previously reported an UHPLC/HRMS method using quadrupole-Orbitrap mass spectrometer in full scan and parallel reaction monitoring (PRM) mode for the detection of 48 AAS and/or their esters in horse hair. However, two injections were required due to the long duty cycle time. In this paper, an UHPLC/HRMS method using multiplexed targeted MS 2 mode was developed and validated to improve the coverage to 65 AAS and/or their esters in a single injection. In addition, a GC/MS/MS method in selected reaction monitoring (SRM) mode was developed to screen for another seven AAS and/or their esters not adequately covered by the UHPLC/HRMS method using the same sample extract after derivatisation with pentafluoropropionic anhydride. The UHPLC/HRMS and GC/MS/MS methods in combination allowed the detection of 72 AAS and/or their esters with estimated limits of detection down to sub to low ppb levels with good interday precision. Method applicability was demonstrated by the detection of boldione and 4-androstenedione in two out-of-competition hair samples and testosterone propionate in a referee hair sample. Copyright © 2018 Elsevier B.V. All rights reserved.

  18. Ultra-high energy physics and standard basic principles

    Directory of Open Access Journals (Sweden)

    Gonzalez-Mestres Luis

    2014-04-01

    Full Text Available It has not yet been elucidated whether the observed flux suppression for ultra-high energy cosmic rays (UHECR at energies above ≃ 4 x 1019 eV is a signature of the Greisen-Zatsepin-Kuzmin (GZK cutoff or a consequence of other phenomena. In both cases, violations of the standard fundamental principles of Physics can be present and play a significant role. They can in particular modify cosmic-ray interactions, propagation or acceleration at very high energy. Thus, in a long-term program, UHECR data can hopefully be used to test relativity, quantum mechanics, energy and momentum conservation, vacuum properties... as well as the elementariness of standard particles. Data on cosmic rays at energies ≃ 1020 eV may also be sensitive to new physics generated well beyond Planck scale. A typical example is provided by the search for possible signatures of a Lorentz symmetry violation (LSV associated to a privileged local reference frame (the "vacuum rest frame", VRF. If a VRF exists, the internal structure of standard particles at ultra-high energy can undergo substantial modifications. Similarly, the conventional particle symmetries may cease to be valid at such energies instead of heading to a grand unification and the structure of vacuum may no longer be governed by standard quantum field theory. Then, the question whether the notion of Planck scale still makes sense clearly becomes relevant and the very grounds of Cosmology can undergo essential modifications. UHECR studies naturally interact with the interpretation of WMAP and Planck observations. Recent Planck data analyses tend to confirm the possible existence of a privileged space direction. If the observed phenomenon turns out to be a signature of the spinorial space-time (SST we suggested in 1996-97, then conventional Particle Physics may correspond to the local properties of standard matter at low enough energy and large enough distances. This would clearly strengthen the cosmological

  19. Advanced Ultra-High Speed Motor for Drilling

    Energy Technology Data Exchange (ETDEWEB)

    Impact Technologies LLC; University of Texas at Arlington

    2007-03-31

    Three (3) designs have been made for two sizes, 6.91 cm (2.72 inch) and 4.29 cm (1.69 inch) outer diameters, of a patented inverted configured Permanent Magnet Synchronous Machines (PMSM) electric motor specifically for drilling at ultra-high rotational speeds (10,000 rpm) and that can utilize advanced drilling methods. Benefits of these motors are stackable power sections, full control (speed and direction) of downhole motors, flow hydraulics independent of motor operation, application of advanced drilling methods (water jetting and abrasive slurry jetting), and the ability of signal/power electric wires through motor(s). Key features of the final designed motors are: fixed non-rotating shaft with stator coils attached; rotating housing with permanent magnet (PM) rotor attached; bit attached to rotating housing; internal channel(s) in a nonrotating shaft; electric components that are hydrostatically isolated from high internal pressure circulating fluids ('muds') by static metal to metal seals; liquid filled motor with smoothed features for minimized turbulence in the motor during operation; and new inverted coated metal-metal hydrodynamic bearings and seals. PMSM, Induction and Switched Reluctance Machines (SRM), all pulse modulated, were considered, but PMSM were determined to provide the highest power density for the shortest motors. Both radial and axial electric PMSM driven motors were designed with axial designs deemed more rugged for ultra-high speed, drilling applications. The 6.91 cm (2.72 inch) OD axial inverted motor can generate 4.18KW (5.61 Hp) power at 10,000 rpm with a 4 Nm (2.95 ft-lbs) of torque for every 30.48 cm (12 inches) of power section. The 6.91 cm (2.72 inch) OD radial inverted motor can generate 5.03 KW (6.74 Hp) with 4.8 Nm (3.54 ft-lb) torque at 10,000 rpm for every 30.48 cm (12 inches) of power section. The 4.29 cm (1.69 inch) OD radial inverted motor can generate 2.56 KW (3.43 Hp) power with 2.44 Nm (1.8 ft-lb) torque at

  20. Spatially resolved chemical analysis of cicada wings using laser-ablation electrospray ionization (LAESI) imaging mass spectrometry (IMS).

    Science.gov (United States)

    Román, Jessica K; Walsh, Callee M; Oh, Junho; Dana, Catherine E; Hong, Sungmin; Jo, Kyoo D; Alleyne, Marianne; Miljkovic, Nenad; Cropek, Donald M

    2018-03-01

    Laser-ablation electrospray ionization (LAESI) imaging mass spectrometry (IMS) is an emerging bioanalytical tool for direct imaging and analysis of biological tissues. Performing ionization in an ambient environment, this technique requires little sample preparation and no additional matrix, and can be performed on natural, uneven surfaces. When combined with optical microscopy, the investigation of biological samples by LAESI allows for spatially resolved compositional analysis. We demonstrate here the applicability of LAESI-IMS for the chemical analysis of thin, desiccated biological samples, specifically Neotibicen pruinosus cicada wings. Positive-ion LAESI-IMS accurate ion-map data was acquired from several wing cells and superimposed onto optical images allowing for compositional comparisons across areas of the wing. Various putative chemical identifications were made indicating the presence of hydrocarbons, lipids/esters, amines/amides, and sulfonated/phosphorylated compounds. With the spatial resolution capability, surprising chemical distribution patterns were observed across the cicada wing, which may assist in correlating trends in surface properties with chemical distribution. Observed ions were either (1) equally dispersed across the wing, (2) more concentrated closer to the body of the insect (proximal end), or (3) more concentrated toward the tip of the wing (distal end). These findings demonstrate LAESI-IMS as a tool for the acquisition of spatially resolved chemical information from fragile, dried insect wings. This LAESI-IMS technique has important implications for the study of functional biomaterials, where understanding the correlation between chemical composition, physical structure, and biological function is critical. Graphical abstract Positive-ion laser-ablation electrospray ionization mass spectrometry coupled with optical imaging provides a powerful tool for the spatially resolved chemical analysis of cicada wings.

  1. LAVA Subsystem Integration and Testing for the RESOLVE Payload of the Resource Prospector Mission: Mass Spectrometers and Gas Chromatography

    Science.gov (United States)

    Coan, Mary R.; Stewart, Elaine M.

    2015-01-01

    The Regolith and Environment Science & Oxygen and Lunar Volatile Extraction (RESOLVE) payload is part of Resource Prospector (RP) along with a rover and a lander that are expected to launch in 2020. RP will identify volatile elements that may be combined and collected to be used for fuel, air, and water in order to enable deeper space exploration. The Resource Prospector mission is a key part of In-Situ Resource Utilization (ISRU). The demand for this method of utilizing resources at the site of exploration is increasing due to the cost of resupply missions and deep space exploration goals. The RESOLVE payload includes the Lunar Advanced Volatile Analysis (LAVA) subsystem. The main instrument used to identify the volatiles evolved from the lunar regolith is the Gas Chromatograph-Mass Spectrometer (GC-MS). LAVA analyzes the volatiles emitted from the Oxygen and Volatile Extraction Node (OVEN) Subsystem. The objective of OVEN is to obtain, weigh, heat and transfer evolved gases to LAVA through the connection between the two subsystems called the LOVEN line. This paper highlights the work completed during a ten week internship that involved the integration, testing, data analysis, and procedure documentation of two candidate mass spectrometers for the LAVA subsystem in order to aid in determining which model to use for flight. Additionally, the examination of data from the integrated Resource Prospector '15 (RP' 15) field test will be presented in order to characterize the amount of water detected from water doped regolith samples.

  2. Resolving mass flux at high spatial and temporal resolution using GRACE intersatellite measurements

    DEFF Research Database (Denmark)

    Rowlands, D. D.; Luthcke, S. B.; Klosko, S. M.

    2005-01-01

    resolution. Using 4° × 4° blocks at 10-day intervals, we estimate the mass of surplus or deficit water over a 52° × 60° grid centered on the Amazon basin for July 2003. We demonstrate that the recovered signals are coherent and correlate well with the expected hydrological signal....... the estimation of static monthly parameters. Through an analysis of the GRACE data residuals, we show that the fundamental temporal and spatial resolution of the GRACE data is 10 days and 400 km. We present an approach similar in concept to altimetric methods that recovers submonthly mass flux at a high spatial...

  3. Ultra-high Density SNParray in Neuroblastoma Molecular Diagnostics

    Directory of Open Access Journals (Sweden)

    Inge M. Ambros

    2014-08-01

    Full Text Available Neuroblastoma serves as a paradigm for applying tumor genomic data for determining patient prognosis and thus for treatment allocation. MYCN status, i.e. amplified vs. non-amplified, was one of the very first biomarkers in oncology to discriminate aggressive from less aggressive or even favorable clinical courses of neuroblastoma. However, MYCN amplification is by far not the only genetic change associated with unfavorable clinical courses: so called segmental chromosomal aberrations, i.e. gains or losses of chromosomal fragments, can also indicate tumor aggressiveness. The clinical use of these genomic aberrations has, however, been hampered for many years by methodical and interpretational problems. Only after reaching worldwide consensus on markers, methodology, and data interpretation, information on SCAs has recently been implemented in clinical studies. Now, a number of collaborative studies within COG, GPOH and SIOPEN use genomic information to stratify therapy for patients with localized and metastatic disease. Recently, new types of DNA based aberrations influencing the clinical behavior of neuroblastomas have been described. Deletions or mutations of genes like ATRX and a phenomenon referred to as chromothripsis are all assumed to correlate with an unfavorable clinical behavior. However, these genomic aberrations need to be scrutinized in larger studies applying the most appropriate techniques. Single nucleotide polymorphism (SNP arrays have proven successful in deciphering genomic aberrations of cancer cells; these techniques, however, are usually not applied in the daily routine. Here, we present an ultra-high density (UHD SNParray technique which is, because of its high specificity and sensitivity and the combined copy number and allele information, highly appropriate for the genomic diagnosis of neuroblastoma and other malignancies.

  4. Properties of matter at ultra-high densities

    International Nuclear Information System (INIS)

    Banerjee, B.; Chitre, S.M.

    1975-01-01

    The recent discovery of pulsars and their subsequent identification with neutron stars has given a great impetus to the study of the behaviour of matter at ultra high densities. The object of these studies is to calculate the equation of state as a function of density. In this paper, the properties of electrically neutral, cold (T=0) matter at unusually high densities has been reviewed. The physics of the equation of state of such matter divides quite naturally in four density ranges. (i) At the very lowest densities the state of minimum energy is a lattice of 56 Fe atoms. This state persists upto 10 7 g/cm 3 . (ii) In the next density region the nuclei at the lattice sites become neutron rich because the high electron Fermi energy makes inverse beta decay possible. (iii) At a density 4.3 x 10 11 the nuclei become so neutron rich that the neutrons start 'dripping' out of the nuclei and form a gas. This density range is characterised by large, neutron-rich nuclei immersed in a neutron gas. (iv) At a density 2.4 x 10 14 g/cm 3 , the nuclei disappear and a fluid of uniform neutron matter with a small percentage of protons and electrons results. The above four density ranges have been discussed in detail as the equation of state is now well established upto the nuclear density 3 x 10 14 g/cm 3 . The problems of extending the equation of state beyond this density are also touched upon. (author)

  5. Diffuse axonal injury at ultra-high field MRI.

    Directory of Open Access Journals (Sweden)

    Christoph Moenninghoff

    Full Text Available Diffuse axonal injury (DAI is a specific type of traumatic brain injury caused by shearing forces leading to widespread tearing of axons and small vessels. Traumatic microbleeds (TMBs are regarded as a radiological marker for DAI. This study aims to compare DAI-associated TMBs at 3 Tesla (T and 7 T susceptibility weighted imaging (SWI to evaluate possible diagnostic benefits of ultra-high field (UHF MRI.10 study participants (4 male, 6 female, age range 20-74 years with known DAI were included. All MR exams were performed with a 3 T MR system (Magnetom Skyra and a 7 T MR research system (Magnetom 7 T, Siemens AG, Healthcare Sector, Erlangen, Germany each in combination with a 32-channel-receive coil. The average time interval between trauma and imaging was 22 months. Location and count of TMBs were independently evaluated by two neuroradiologists on 3 T and 7 T SWI images with similar and additionally increased spatial resolution at 7 T. Inter- and intraobserver reliability was assessed using the interclass correlation coefficient (ICC. Count and diameter of TMB were evaluated with Wilcoxon signed rank test.Susceptibility weighted imaging revealed a total of 485 TMBs (range 1-190, median 25 at 3 T, 584 TMBs (plus 20%, range 1-262, median 30.5 at 7 T with similar spatial resolution, and 684 TMBs (plus 41%, range 1-288, median 39.5 at 7 T with 10-times higher spatial resolution. Hemorrhagic DAI appeared significantly larger at 7 T compared to 3 T (p = 0.005. Inter- and intraobserver correlation regarding the counted TMB was high and almost equal 3 T and 7 T.7 T SWI improves the depiction of small hemorrhagic DAI compared to 3 T and may be supplementary to lower field strengths for diagnostic in inconclusive or medicolegal cases.

  6. Properties of crosslinked ultra-high-molecular-weight polyethylene.

    Science.gov (United States)

    Lewis, G

    2001-02-01

    Substantially reducing the rate of generation of wear particles at the surfaces of ultra-high-molecular-weight polyethylene (UHMWPE) orthopedic implant bearing components, in vivo, is widely regarded as one of the most formidable challenges in modern arthroplasty. In the light of this, much research attention has been paid to the myriad of endogenous and exogenous factors that have been postulated to affect this wear rate, one such factor being the polymer itself. In recent years, there has been a resurgence of interest in crosslinking the polymer as a way of improving its properties that are considered relevant to its use for fabricating bearing components. Such properties include wear resistance, fatigue life, and fatigue crack propagation rate. Although a large volume of literature exists on the topic on the impact of crosslinking on the properties of UHMWPE, no critical appraisal of this literature has been published. This is one of the goals of the present article, which emphasizes three aspects. The first is the trade-off between improvement in wear resistance and depreciation in other mechanical and physical properties. The second aspect is the presentation of a method of estimating the optimal value of a crosslinking process variable (such as dose in radiation-induced crosslinking) that takes into account this trade-off. The third aspect is the description of a collection of under- and unexplored research areas in the field of crosslinked UHMWPE, such as the role of starting resin on the properties of the crosslinked polymer, and the in vitro evaluation of the wear rate of crosslinked tibial inserts and other bearing components that, in vivo, are subjected to nearly unidirectional motion.

  7. Near-Field Cosmology with Resolved Stellar Populations Around Local Volume LMC Stellar-Mass Galaxies

    Science.gov (United States)

    Carlin, Jeffrey L.; Sand, David J.; Willman, Beth; Brodie, Jean P.; Crnojevic, Denija; Forbes, Duncan; Hargis, Jonathan R.; Peter, Annika; Pucha, Ragadeepika; Romanowsky, Aaron J.; Spekkens, Kristine; Strader, Jay

    2018-06-01

    We discuss our ongoing observational program to comprehensively map the entire virial volumes of roughly LMC stellar mass galaxies at distances of ~2-4 Mpc. The MADCASH (Magellanic Analog Dwarf Companions And Stellar Halos) survey will deliver the first census of the dwarf satellite populations and stellar halo properties within LMC-like environments in the Local Volume. Our results will inform our understanding of the recent DES discoveries of dwarf satellites tentatively affiliated with the LMC/SMC system. This program has already yielded the discovery of the faintest known dwarf galaxy satellite of an LMC stellar-mass host beyond the Local Group, based on deep Subaru+HyperSuprimeCam imaging reaching ~2 magnitudes below its TRGB, and at least two additional candidate satellites. We will summarize the survey results and status to date, highlighting some challenges encountered and lessons learned as we process the data for this program through a prototype LSST pipeline. Our program will examine whether LMC stellar mass dwarfs have extended stellar halos, allowing us to assess the relative contributions of in-situ stars vs. merger debris to their stellar populations and halo density profiles. We outline the constraints on galaxy formation models that will be provided by our observations of low-mass galaxy halos and their satellites.

  8. ON ULTRA-HIGH-ENERGY COSMIC RAYS AND THEIR RESULTANT GAMMA-RAYS

    Energy Technology Data Exchange (ETDEWEB)

    Gavish, Eyal; Eichler, David [Physics Department, Ben-Gurion University, Be’er-Sheva 84105 (Israel)

    2016-05-01

    The Fermi Large Area Telescope collaboration has recently reported on 50 months of measurements of the isotropic extragalactic gamma-ray background (EGRB) spectrum between 100 MeV and 820 GeV. Ultra-high-energy cosmic ray (UHECR) protons interact with the cosmic microwave background photons and produce cascade photons of energies 10 MeV–1 TeV that contribute to the EGRB flux. We examine seven possible evolution models for UHECRs and find that UHECR sources that evolve as the star formation rate (SFR), medium low luminosity active galactic nuclei type-1 ( L = 10{sup 43.5} erg s{sup −1} in the [0.5–2] KeV band), and BL Lacertae objects (BL Lacs) are the most acceptable given the constraints imposed by the observed EGRB. Other possibilities produce too much secondary γ -radiation. In all cases, the decaying dark matter (DM) contribution improves the fit at high energy, but the contribution of still unresolved blazars, which would leave the smallest role for decaying DM, may yet provide an alternative improvement. The possibility that the entire EGRB can be fitted with resolvable but not-yet-resolved blazars, as recently claimed by Ajello et al., would leave little room in the EGRB to accommodate γ -rays from extragalactic UHECR production, even for many source evolution rates that would otherwise be acceptable. We find that under the assumption of UHECRs being mostly protons, there is not enough room for producing extragalactic UHECRs with active galactic nucleus, gamma-ray burst, or even SFR source evolution. Sources that evolve as BL Lacs, on the other hand, would produce much less secondary γ -radiation and would remain a viable source of UHECRs, provided that they dominate.

  9. Development of data communication system with ultra high frequency radio wave for implantable artificial hearts.

    Science.gov (United States)

    Tsujimura, Shinichi; Yamagishi, Hiroto; Sankai, Yoshiyuki

    2009-01-01

    In order to minimize infection risks of patients with artificial hearts, wireless data transmission methods with electromagnetic induction or light have been developed. However, these methods tend to become difficult to transmit data if the external data transmission unit moves from its proper position. To resolve this serious problem, the purpose of this study is to develop a prototype wireless data communication system with ultra high frequency radio wave and confirm its performance. Due to its high-speed communication rate, low power consumption, high tolerance to electromagnetic disturbances, and secure wireless communication, we adopted Bluetooth radio wave technology for our system. The system consists of an internal data transmission unit and an external data transmission unit (53 by 64 by 16 mm, each), and each has a Bluetooth module (radio field intensity: 4 dBm, receiver sensitivity: -80 dBm). The internal unit also has a micro controller with an 8-channel 10-bit A/D converter, and the external unit also has a RS-232C converter. We experimented with the internal unit implanted into pig meat, and carried out data transmission tests to evaluate the performance of this system in tissue thickness of up to 3 mm. As a result, data transfer speeds of about 20 kbps were achieved within the communication distance of 10 m. In conclusion, we confirmed that the system can wirelessly transmit the data from the inside of the body to the outside, and it promises to resolve unstable data transmission due to accidental movements of an external data transmission unit.

  10. Single-event transient imaging with an ultra-high-speed temporally compressive multi-aperture CMOS image sensor.

    Science.gov (United States)

    Mochizuki, Futa; Kagawa, Keiichiro; Okihara, Shin-ichiro; Seo, Min-Woong; Zhang, Bo; Takasawa, Taishi; Yasutomi, Keita; Kawahito, Shoji

    2016-02-22

    In the work described in this paper, an image reproduction scheme with an ultra-high-speed temporally compressive multi-aperture CMOS image sensor was demonstrated. The sensor captures an object by compressing a sequence of images with focal-plane temporally random-coded shutters, followed by reconstruction of time-resolved images. Because signals are modulated pixel-by-pixel during capturing, the maximum frame rate is defined only by the charge transfer speed and can thus be higher than those of conventional ultra-high-speed cameras. The frame rate and optical efficiency of the multi-aperture scheme are discussed. To demonstrate the proposed imaging method, a 5×3 multi-aperture image sensor was fabricated. The average rising and falling times of the shutters were 1.53 ns and 1.69 ns, respectively. The maximum skew among the shutters was 3 ns. The sensor observed plasma emission by compressing it to 15 frames, and a series of 32 images at 200 Mfps was reconstructed. In the experiment, by correcting disparities and considering temporal pixel responses, artifacts in the reconstructed images were reduced. An improvement in PSNR from 25.8 dB to 30.8 dB was confirmed in simulations.

  11. Time resolved mass flow measurements for a fast gas delivery system

    International Nuclear Information System (INIS)

    Ruden, E.L.; Degnan, J.H.; Hussey, T.W.; Scott, M.C.; Graham, J.D.; Coffey, S.K.

    1992-01-01

    A technique is demonstrated whereby the delivered mass and flow rate vs. time of a short rise time gas delivery system may be accurately determined. The gas mass M which flows past a point in a gas delivery system by an arbitrary time t may be accurately measured if that point is sealed off within a time interval short compared to the mass flow time scale. If the ejected mass is allowed to equilibrate in a known volume after being cut off from its source, a conventional static pressure measurement before and after injection, and application of the ideal gas law suffices. Assuming reproducibility, a time history M(t) may be generated, allowing the flow rate vs. time dM(t)/dt to be determined. Mass flow measurements are presented for a fast delivery system in which the flow of argon through a 3.2 mm I.D., 0.76 mm thick copper tube is cut off by imploding (θ pinching) the tube using a single turn tungsten magnetic field coil. Pinch discharge parameters are 44 μf, 20 kV, 47 nH, 3.5 mΩ, 584 kA, and 8.63 ps current period. Optical measurements of the tube's internal area vs. time indicate that the tube is sealed 2 ps from the time the tube is still 90% open (7 μs from the start of pinch current). The pinch delay is varied from 500--1,500 ps from the valve trigger (0--1,000 ps from the start of gas flow). The mass injected into the test volume is ∼ 100 μg during this interval. The leak rate of the sealed tube results in a mass increase of only ∼ 0.1 μg by the time the pressure gauge stabilizes (6 s). Results are correlated with piezoelectric probe measurements of the gas flow and 2-D axisymmetric numerical simulations of the θ pinch process. Simulations of a θ pinch suitable for characterizing an annular supersonic nozzle typical of those used in gas puff z pinches are discussed

  12. Spatially resolved δ13C analysis using laser ablation isotope ratio mass spectrometry

    Science.gov (United States)

    Moran, J.; Riha, K. M.; Nims, M. K.; Linley, T. J.; Hess, N. J.; Nico, P. S.

    2014-12-01

    Inherent geochemical, organic matter, and microbial heterogeneity over small spatial scales can complicate studies of carbon dynamics through soils. Stable isotope analysis has a strong history of helping track substrate turnover, delineate rhizosphere activity zones, and identifying transitions in vegetation cover, but most traditional isotope approaches are limited in spatial resolution by a combination of physical separation techniques (manual dissection) and IRMS instrument sensitivity. We coupled laser ablation sampling with isotope measurement via IRMS to enable spatially resolved analysis over solid surfaces. Once a targeted sample region is ablated the resulting particulates are entrained in a helium carrier gas and passed through a combustion reactor where carbon is converted to CO2. Cyrotrapping of the resulting CO2 enables a reduction in carrier gas flow which improves overall measurement sensitivity versus traditional, high flow sample introduction. Currently we are performing sample analysis at 50 μm resolution, require 65 ng C per analysis, and achieve measurement precision consistent with other continuous flow techniques. We will discuss applications of the laser ablation IRMS (LA-IRMS) system to microbial communities and fish ecology studies to demonstrate the merits of this technique and how similar analytical approaches can be transitioned to soil systems. Preliminary efforts at analyzing soil samples will be used to highlight strengths and limitations of the LA-IRMS approach, paying particular attention to sample preparation requirements, spatial resolution, sample analysis time, and the types of questions most conducive to analysis via LA-IRMS.

  13. Time-resolved pulsed hydrogen/deuterium exchange mass spectrometry probes gaseous proteins structural kinetics.

    Science.gov (United States)

    Rajabi, Khadijeh

    2015-01-01

    A pulsed hydrogen/deuterium exchange (HDX) method has been developed for rapid monitoring of the exchange kinetics of protein ions with D2O a few milliseconds after electrospray ionization (ESI). The stepwise gradual evolution of HDX of multiply charged protein ions was monitored using the pulsed HDX mass spectrometry technique. Upon introducing a very short pulse of D2O (in the μs to ms time scale) into the linear ion trap (LIT) of a time-of-flight (TOF) mass spectrometer, bimodal distributions were detected for the ions of cytochrome c and ubiquitin. Mechanistic details of HDX reactions for ubiquitin and cytochrome c in the gas phase were uncovered and the structural transitions were followed by analyzing the kinetics of HDX.

  14. Hybrid method to resolve the neutrino mass hierarchy by supernova (anti)neutrino induced reactions

    Energy Technology Data Exchange (ETDEWEB)

    Vale, D. [Department of Physics, Faculty of Science, University of Zagreb, Bijenička c. 32, HR-10000 Zagreb (Croatia); Rauscher, T. [Centre for Astrophysics Research, University of Hertfordshire, College Lane, Hatfield AL10 9AB (United Kingdom); Paar, N., E-mail: dvale@phy.hr, E-mail: Thomas.Rauscher@unibas.ch, E-mail: npaar@phy.hr [Department of Physics, University of Basel, Klingelbergstrasse 82, CH-4056 Basel (Switzerland)

    2016-02-01

    We introduce a hybrid method to determine the neutrino mass hierarchy by simultaneous measurements of responses of at least two detectors to antineutrino and neutrino fluxes from accretion and cooling phases of core-collapse supernovae. The (anti)neutrino-nucleus cross sections for {sup 56}Fe and {sup 208}Pb are calculated in the framework of the relativistic nuclear energy density functional and weak interaction Hamiltonian, while the cross sections for inelastic scattering on free protons p(ν-bar {sub e},e{sup +})n are obtained using heavy-baryon chiral perturbation theory. The modelling of (anti)neutrino fluxes emitted from a protoneutron star in a core-collapse supernova include collective and Mikheyev-Smirnov-Wolfenstein effects inside the exploding star. The particle emission rates from the elementary decay modes of the daughter nuclei are calculated for normal and inverted neutrino mass hierarchy. It is shown that simultaneous use of (anti)neutrino detectors with different target material allows to determine the neutrino mass hierarchy from the ratios of ν{sub e}- and ν-bar {sub e}-induced particle emissions. This hybrid method favors neutrinos from the supernova cooling phase and the implementation of detectors with heavier target nuclei ({sup 208}Pb) for the neutrino sector, while for antineutrinos the use of free protons in mineral oil or water is the appropriate choice.

  15. Hybrid method to resolve the neutrino mass hierarchy by supernova (anti)neutrino induced reactions

    Science.gov (United States)

    Vale, D.; Rauscher, T.; Paar, N.

    2016-02-01

    We introduce a hybrid method to determine the neutrino mass hierarchy by simultaneous measurements of responses of at least two detectors to antineutrino and neutrino fluxes from accretion and cooling phases of core-collapse supernovae. The (anti)neutrino-nucleus cross sections for 56Fe and 208Pb are calculated in the framework of the relativistic nuclear energy density functional and weak interaction Hamiltonian, while the cross sections for inelastic scattering on free protons p(bar nue,e+)n are obtained using heavy-baryon chiral perturbation theory. The modelling of (anti)neutrino fluxes emitted from a protoneutron star in a core-collapse supernova include collective and Mikheyev-Smirnov-Wolfenstein effects inside the exploding star. The particle emission rates from the elementary decay modes of the daughter nuclei are calculated for normal and inverted neutrino mass hierarchy. It is shown that simultaneous use of (anti)neutrino detectors with different target material allows to determine the neutrino mass hierarchy from the ratios of νe- and bar nue-induced particle emissions. This hybrid method favors neutrinos from the supernova cooling phase and the implementation of detectors with heavier target nuclei (208Pb) for the neutrino sector, while for antineutrinos the use of free protons in mineral oil or water is the appropriate choice.

  16. Acoustic detection of ultra-high energy cascades in ice

    Energy Technology Data Exchange (ETDEWEB)

    Boeser, S.

    2006-12-08

    Current underwater optical neutrino telescopes are designed to detect neutrinos from astrophysical sources with energies in the TeV range. Due to the low fluxes and small cross sections, no high energy neutrinos of extraterrestrial origin have been observed so far. Only the Cherenkov neutrino detectors on the km{sup 3} scale that are currently under construction will have the necessary volume to observe these rare interactions. For the guaranteed source of neutrinos from interactions of the ultra-high energy cosmic at EeV energies rays with the ambient cosmic microwave background, event rates of only one per year are expected in these experiments. To measure the flux and verify the predicted cross sections of these cosmogenic neutrinos, an observed volume of the order of 100 km{sup 3} will be necessary, that will not be feasible with existing detection techniques. Alternative methods are required to build a detector on these scales. One promising idea is to record the acoustic waves generated in hadronic or electromagnetic cascades following the neutrino interaction. The higher amplitudes of the sonic signal and the large expected absorption length of sound favour South Polar ice instead of sea water as a medium. The prerequisites for an estimate of the potential of such a detector are suitable acoustic sensors, a verification of the model of thermo-acoustic sound generation and a determination of the acoustic properties of the ice. In a theoretical derivation the mechanism of thermo-elastic excitation of acoustic waves was shown to be equivalent for isotropic solids and liquids. Following a detailed analysis of the existing knowledge a simulation study of a hybrid optical-radio-acoustic detector has been performed. Ultrasonic sensors dedicated to in-ice application were developed and have been used to record acoustic signals from intense proton and laser beams in water and ice. With the obtained experience, the hitherto largest array of acoustic sensors and

  17. Ultra-high-energy cosmic rays from radio galaxies

    Science.gov (United States)

    Eichmann, B.; Rachen, J. P.; Merten, L.; van Vliet, A.; Becker Tjus, J.

    2018-02-01

    Radio galaxies are intensively discussed as the sources of cosmic rays observed above about 3 × 1018 eV, called ultra-high energy cosmic rays (UHECRs). We present a first, systematic approach that takes the individual characteristics of these sources into account, as well as the impact of the extragalactic magnetic-field structures up to a distance of 120 Mpc. We use a mixed simulation setup, based on 3D simulations of UHECRs ejected by observed, individual radio galaxies taken out to a distance of 120 Mpc, and on 1D simulations over a continuous source distribution contributing from beyond 120 Mpc. Additionally, we include the ultra-luminous radio galaxy Cygnus A at a distance of about 250 Mpc, as its contribution is so strong that it must be considered as an individual point source. The implementation of the UHECR ejection in our simulation setup, both that of individual radio galaxies and the continuous source function, is based on a detailed consideration of the physics of radio jets and standard first-order Fermi acceleration. This allows to derive the spectrum of ejected UHECR as a function of radio luminosity, and at the same time provides an absolute normalization of the problem involving only a small set of parameters adjustable within narrow constraints. We show that the average contribution of radio galaxies taken over a very large volume cannot explain the observed features of UHECRs measured at Earth. However, we obtain excellent agreement with the spectrum, composition, and arrival-direction distribution of UHECRs measured by the Pierre Auger Observatory, if we assume that most UHECRs observed arise from only two sources: the ultra-luminous radio galaxy Cygnus A, providing a mostly light composition of nuclear species dominating up to about 6 × 1019 eV, and the nearest radio galaxy Centaurus A, providing a heavy composition dominating above 6 × 1019 eV . Here we have to assume that extragalactic magnetic fields out to 250 Mpc, which we did not

  18. Acoustic detection of ultra-high energy cascades in ice

    International Nuclear Information System (INIS)

    Boeser, S.

    2006-01-01

    Current underwater optical neutrino telescopes are designed to detect neutrinos from astrophysical sources with energies in the TeV range. Due to the low fluxes and small cross sections, no high energy neutrinos of extraterrestrial origin have been observed so far. Only the Cherenkov neutrino detectors on the km 3 scale that are currently under construction will have the necessary volume to observe these rare interactions. For the guaranteed source of neutrinos from interactions of the ultra-high energy cosmic at EeV energies rays with the ambient cosmic microwave background, event rates of only one per year are expected in these experiments. To measure the flux and verify the predicted cross sections of these cosmogenic neutrinos, an observed volume of the order of 100 km 3 will be necessary, that will not be feasible with existing detection techniques. Alternative methods are required to build a detector on these scales. One promising idea is to record the acoustic waves generated in hadronic or electromagnetic cascades following the neutrino interaction. The higher amplitudes of the sonic signal and the large expected absorption length of sound favour South Polar ice instead of sea water as a medium. The prerequisites for an estimate of the potential of such a detector are suitable acoustic sensors, a verification of the model of thermo-acoustic sound generation and a determination of the acoustic properties of the ice. In a theoretical derivation the mechanism of thermo-elastic excitation of acoustic waves was shown to be equivalent for isotropic solids and liquids. Following a detailed analysis of the existing knowledge a simulation study of a hybrid optical-radio-acoustic detector has been performed. Ultrasonic sensors dedicated to in-ice application were developed and have been used to record acoustic signals from intense proton and laser beams in water and ice. With the obtained experience, the hitherto largest array of acoustic sensors and transmitters was

  19. Comprehensive analysis of Polygoni Multiflori Radix of different geographical origins using ultra-high-performance liquid chromatography fingerprints and multivariate chemometric methods

    Directory of Open Access Journals (Sweden)

    Li-Li Sun

    2018-01-01

    Full Text Available Polygoni Multiflori Radix (PMR is increasingly being used not just as a traditional herbal medicine but also as a popular functional food. In this study, multivariate chemometric methods and mass spectrometry were combined to analyze the ultra-high-performance liquid chromatograph (UPLC fingerprints of PMR from six different geographical origins. A chemometric strategy based on multivariate curve resolution–alternating least squares (MCR–ALS and three classification methods is proposed to analyze the UPLC fingerprints obtained. Common chromatographic problems, including the background contribution, baseline contribution, and peak overlap, were handled by the established MCR–ALS model. A total of 22 components were resolved. Moreover, relative species concentrations were obtained from the MCR–ALS model, which was used for multivariate classification analysis. Principal component analysis (PCA and Ward's method have been applied to classify 72 PMR samples from six different geographical regions. The PCA score plot showed that the PMR samples fell into four clusters, which related to the geographical location and climate of the source areas. The results were then corroborated by Ward's method. In addition, according to the variance-weighted distance between cluster centers obtained from Ward's method, five components were identified as the most significant variables (chemical markers for cluster discrimination. A counter-propagation artificial neural network has been applied to confirm and predict the effects of chemical markers on different samples. Finally, the five chemical markers were identified by UPLC–quadrupole time-of-flight mass spectrometer. Components 3, 12, 16, 18, and 19 were identified as 2,3,5,4′-tetrahydroxy-stilbene-2-O-β-d-glucoside, emodin-8-O-β-d-glucopyranoside, emodin-8-O-(6′-O-acetyl-β-d-glucopyranoside, emodin, and physcion, respectively. In conclusion, the proposed method can be applied for the

  20. Resolving neutrino mass hierarchy from supernova (anti)neutrino-nucleus reactions

    Science.gov (United States)

    Vale, Deni; Paar, Nils

    2015-10-01

    Recently a hybrid method has been introduced to determine neutrino mass hierarchy by simultaneous measurements of detector responses induced by antineutrino and neutrino fluxes from accretion and cooling phase of type II supernova. The (anti)neutrino-nucleus cross sections for 12C, 16O, 56Fe and 208Pb are calculated in the framework of relativistic nuclear energy density functional and weak interaction Hamiltonian, while the cross sections for inelastic scattering on free protons in mineral oil and water, p (v¯e,e+)n are obtained using heavy-baryon chiral perturbation theory. The simulations of (anti)neutrino fluxes emitted from a proto-neutron star in a core-collapse supernova include collective and Mikheyev-Smirnov-Wolfenstein effects inside star. It is shown that simultaneous use of ve/v¯e detectors with different target material allow to determine the neutrino mass hierarchy from the ratios of ve/v¯e induced particle emissions. The hybrid method favors detectors with heavier target nuclei (208Pb) for the neutrino sector, while for antineutrinos the use of free protons in mineral oil and water is more appropriate.

  1. Enantioseparation of dansyl amino acids by ultra-high pressure liquid chromatography using cationic β-cyclodextrins as chiral additives.

    Science.gov (United States)

    Xiao, Yin; Tan, Timothy Thatt Yang; Ng, Siu-Choon

    2011-04-07

    This work reports the application of ultra-high pressure liquid chromatography (UHPLC) for reasonably fast enantiorecognition of some dansyl amino acids by employing three cationic β-cyclodextrins (β-CDs) as chiral additives. Good resolutions were obtained on an Agilent C18 column (2.1 mm i.d.; 1.8 μm; 50 mm length) with 1% (v/v) triethylammonium acetate buffered at pH 4.7 and acetonitrile as the mobile phase. Most of the analytes could be baseline resolved within 10 min. Increased cationic CD concentration or acetonitrile proportion in the mobile phase results in a decreased retention factor but accentuated selectivity. Furthermore, molecular mechanics calculation was performed and found to be consistent with the experimental results. © The Royal Society of Chemistry 2011

  2. Innovative Ultra-High Efficiency Cryogenic Actuators for Rocket Test Facilities, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — The SBIR Phase I project will develop advanced ultra-high efficiency cryogenic actuators for NASA cryogenic fluid transfer application. The actuator will have low...

  3. Failure Modes of a Unidirectional Ultra-High-Modulus Carbon-Fiber/Carbon-Matrix Composite

    National Research Council Canada - National Science Library

    Zaldivar, R

    1998-01-01

    The objective of this study was to observe the effects of various microstructural features on the in situ, room-temperature tensile fracture behavior of an ultra-high-modulus, unidirectional carbon/carbon (C/C...

  4. Probing physics at extreme energies with cosmic ultra-high energy ...

    Indian Academy of Sciences (India)

    testing new particle physics. Keywords. Ultra-high ... conventional theories of CR origin based on acceleration of charged particles in powerful ... Before discussing specific scenarios for UHECR origin we give a short account of the numerical ...

  5. Ultra-high performance concrete : a state-of-the-art report for the bridge community.

    Science.gov (United States)

    2013-06-01

    "The term Ultra-High Performance Concrete (UHPC) refers to a relatively new class of advanced cementitious : composite materials whose mechanical and durability properties far surpass those of conventional concrete. This : class of concrete has been ...

  6. Design and evaluation of a single-span bridge using ultra-high performance concrete.

    Science.gov (United States)

    2009-09-01

    "Research presented herein describes an application of a newly developed material called Ultra-High Performance Concrete (UHPC) to a : single-span bridge. The two primary objectives of this research were to develop a shear design procedure for possib...

  7. Durability and smart condition assessment of ultra-high performance concrete in cold climates.

    Science.gov (United States)

    2016-12-31

    The goals of this study were to develop ecological ultra-high performance concrete (UHPC) with local materials and supplementary cementitious materials and to evaluate the long-term performance of UHPC in cold climates using effective mechanical test...

  8. Time resolved investigations on biogenic trace gases exchanges using proton-transfer-reaction mass spectrometry

    International Nuclear Information System (INIS)

    Karl, T.

    2000-02-01

    Volatile organic compounds (VOCs) released from vegetation, including wound-induced VOCs, can have important effects on atmospheric chemistry. The analytical methods for measuring wound-induced VOCs, especially the hexenal family of VOCs (hexenals, hexenols and hexenyl esters) but also compounds like acetaldehyde, are complicated by their chemical instability and the transient nature of their formation after leaf and stem wounding. The goal of this thesis was to assess, quantify and complement our understanding on the origin of tropospheric VOCs. This thesis demonstrates that formation and emission of hexenal family compounds can be monitored on-line using proton-transfer-reaction mass spectrometry (PTR-MS), avoiding the need for preconcentration or chromatography. These measurements revealed the rapid emission of the parent compound, (Z)-3-hexenal, within 1-2 seconds of wounding of leaves from various woody and nonwoody plants, and its metabolites including (E)-2-hexenal, hexenols and hexenyl acetates. Emission of (Z)-3-hexenal from detached, drying leaves averaged 500 μg (gram dry weight)-1. PTR-MS showed to be a useful tool for the analysis of VOC emissions resulting from grazing, herbivory, harvesting and senescing leaves. The release of reactive VOCs during lawn mowing was observed in on-line ambient air measurements in July and August 1998 in the outskirts of Innsbruck. Also obtained were data on emission rates of reactive aldehydes (hexenyl compounds) and other abundant VOCs such as methanol, acetaldehyde and acetone from drying grass in various chamber experiments. Fluxes were measured after cutting of grass using eddy covariance measurements and the micrometeorological gradient method (Obhukov-Similarity-Method). Comparison of data obtained by these different methods showed satisfactory agreement. The highest fluxes for methanol during drying were 5 mg/m2h, for (Z)-3-hexenal 1.5 mg/m2h. Experiments conducted on the Sonnblick Observatory in Fall and Winter

  9. The Time Lens Concept Applied to Ultra-High-Speed OTDM Signal Processing

    DEFF Research Database (Denmark)

    Clausen, Anders; Palushani, Evarist; Mulvad, Hans Christian Hansen

    2013-01-01

    This survey paper presents some of the applications where the versatile time-lens concept successfully can be applied to ultra-high-speed serial systems by offering expected needed functionalities for future optical communication networks.......This survey paper presents some of the applications where the versatile time-lens concept successfully can be applied to ultra-high-speed serial systems by offering expected needed functionalities for future optical communication networks....

  10. SimProp: a simulation code for ultra high energy cosmic ray propagation

    International Nuclear Information System (INIS)

    Aloisio, R.; Grillo, A.F.; Boncioli, D.; Petrera, S.; Salamida, F.

    2012-01-01

    A new Monte Carlo simulation code for the propagation of Ultra High Energy Cosmic Rays is presented. The results of this simulation scheme are tested by comparison with results of another Monte Carlo computation as well as with the results obtained by directly solving the kinetic equation for the propagation of Ultra High Energy Cosmic Rays. A short comparison with the latest flux published by the Pierre Auger collaboration is also presented

  11. Laser beam welding of new ultra-high strength and supra-ductile steels

    OpenAIRE

    Dahmen, M.

    2015-01-01

    Ultra-high strength and supra-ductile are entering fields of new applications. Those materials are excellent candidates for modern light-weight construction and functional integration. As ultra-high strength steels the stainless martensitic grade 1.4034 and the bainitic steel UNS 53835 are investigated. For the supra-ductile steels stand two high austenitic steels with 18 and 28 % manganese. As there are no processing windows an approach from the metallurgical base on is required. Adjusting t...

  12. Connections in Precast Buildings using Ultra High-Strength Fibre Reinforced Concrete

    DEFF Research Database (Denmark)

    Hansen, Lars Pilegaard

    1995-01-01

    Ultra high-strength concrete adds new dimensions to the design of concrete structures. It is a brittle material but introducing fibres into the matrix changes the material into a highly ductile material. Furthermore, the fibre reinforcement increases the anchorage of traditional reinforcement bar...... and the fire resistance. Such a fibre reinforced ultra high-strength material has been used to develop a simple joint solution between slab elements in a column - slab building system....

  13. Is Episodic Accretion Necessary to Resolve the Luminosity Problem in Low-Mass Protostars?

    Science.gov (United States)

    Sevrinsky, Raymond Andrew; Dunham, Michael

    2017-01-01

    In this contribution, we compare the results of protostellar accretion simulations for scenarios both containing and lacking episodic accretion activity. We determine synthetic observational signatures for collapsing protostars by taking hydrodynamical simulations predicting highly variable episodic accretion events, filtering out the stochastic behavior by applying power law fits to the mass accretion rates onto the disk and central star, and using the filtered rates as inputs to two-dimensional radiative transfer calculations. The spectral energy distributions generated by these calculations are used to calculate standard observational signatures of Lbol and Tbol, and compared directly to a sample of 230 embedded protostars. We explore the degree to which these continually declining accretion models successfully reproduce the observed spread of protostellar luminosities, and examine their consistency with the prior variable models to investigate the degree to which episodic accretion bursts are necessary in protostellar formation theories to match observations of field protostars. The SAO REU program is funded in part by the National Science Foundation REU and Department of Defense ASSURE programs under NSF Grant no. 1262851, and by the Smithsonian Institution.

  14. Design Strategies for Ultra-high Efficiency Photovoltaics

    Science.gov (United States)

    Warmann, Emily Cathryn

    While concentrator photovoltaic cells have shown significant improvements in efficiency in the past ten years, once these cells are integrated into concentrating optics, connected to a power conditioning system and deployed in the field, the overall module efficiency drops to only 34 to 36%. This efficiency is impressive compared to conventional flat plate modules, but it is far short of the theoretical limits for solar energy conversion. Designing a system capable of achieving ultra high efficiency of 50% or greater cannot be achieved by refinement and iteration of current design approaches. This thesis takes a systems approach to designing a photovoltaic system capable of 50% efficient performance using conventional diode-based solar cells. The effort began with an exploration of the limiting efficiency of spectrum splitting ensembles with 2 to 20 sub cells in different electrical configurations. Incorporating realistic non-ideal performance with the computationally simple detailed balance approach resulted in practical limits that are useful to identify specific cell performance requirements. This effort quantified the relative benefit of additional cells and concentration for system efficiency, which will help in designing practical optical systems. Efforts to improve the quality of the solar cells themselves focused on the development of tunable lattice constant epitaxial templates. Initially intended to enable lattice matched multijunction solar cells, these templates would enable increased flexibility in band gap selection for spectrum splitting ensembles and enhanced radiative quality relative to metamorphic growth. The III-V material family is commonly used for multijunction solar cells both for its high radiative quality and for the ease of integrating multiple band gaps into one monolithic growth. The band gap flexibility is limited by the lattice constant of available growth templates. The virtual substrate consists of a thin III-V film with the desired

  15. SDSS-IV MaNGA: The Spatially Resolved Stellar Initial Mass Function in ˜400 Early-Type Galaxies

    Science.gov (United States)

    Parikh, Taniya; Thomas, Daniel; Maraston, Claudia; Westfall, Kyle B.; Goddard, Daniel; Lian, Jianhui; Meneses-Goytia, Sofia; Jones, Amy; Vaughan, Sam; Andrews, Brett H.; Bershady, Matthew; Bizyaev, Dmitry; Brinkmann, Jonathan; Brownstein, Joel R.; Bundy, Kevin; Drory, Niv; Emsellem, Eric; Law, David R.; Newman, Jeffrey A.; Roman-Lopes, Alexandre; Wake, David; Yan, Renbin; Zheng, Zheng

    2018-03-01

    MaNGA provides the opportunity to make precise spatially resolved measurements of the IMF slope in galaxies owing to its unique combination of spatial resolution, wavelength coverage and sample size. We derive radial gradients in age, element abundances and IMF slope analysing optical and near-infrared absorption features from stacked spectra out to the half-light radius of 366 early-type galaxies with masses 9.9 - 10.8 log M/M⊙. We find flat gradients in age and [α/Fe] ratio, as well as negative gradients in metallicity, consistent with the literature. We further derive significant negative gradients in the [Na/Fe] ratio with galaxy centres being well enhanced in Na abundance by up to 0.5 dex. Finally, we find a gradient in IMF slope with a bottom-heavy IMF in the centre (typical mass excess factor of 1.5) and a Milky Way-type IMF at the half-light radius. This pattern is mass-dependent with the lowest mass galaxies in our sample featuring only a shallow gradient around a Milky Way IMF. Our results imply the local IMF-σ relation within galaxies to be even steeper than the global relation and hint towards the local metallicity being the dominating factor behind the IMF variations. We also employ different stellar population models in our analysis and show that a radial IMF gradient is found independently of the stellar population model used. A similar analysis of the Wing-Ford band provides inconsistent results and further evidence of the difficulty in measuring and modelling this particular feature.

  16. SPATIALLY RESOLVED OBSERVATIONS OF THE BIPOLAR OPTICAL OUTFLOW FROM THE BROWN DWARF 2MASS J12073347–3932540

    International Nuclear Information System (INIS)

    Whelan, E. T.; Ray, T. P.; Comeron, F.; Bacciotti, F.; Kavanagh, P. J.

    2012-01-01

    Studies of brown dwarf (BD) outflows provide information pertinent to questions on BD formation, as well as allowing outflow mechanisms to be investigated at the lowest masses. Here new observations of the bipolar outflow from the 24 M JUP BD 2MASS J12073347–3932540 are presented. The outflow was originally identified through the spectro-astrometric analysis of the [O I]λ6300 emission line. Follow-up observations consisting of spectra and [S II], R-band and I-band images were obtained. The new spectra confirm the original results and are used to constrain the outflow position angle (P.A.) at ∼65°. The [O I]λ6300 emission line region is spatially resolved and the outflow is detected in the [S II] images. The detection is firstly in the form of an elongation of the point-spread function (PSF) along the direction of the outflow P.A. Four faint knot-like features (labeled A-D) are also observed to the southwest of 2MASS J12073347–3932540 along the same P.A. suggested by the spectra and the elongation in the PSF. Interestingly, D, the feature furthest from the source, is bow shaped with the apex pointing away from 2MASS J12073347–3932540. A color-color analysis allows us to conclude that at least feature D is part of the outflow under investigation while A is likely a star or galaxy. Follow-up observations are needed to confirm the origin of B and C. This is a first for a BD, as BD optical outflows have to date only been detected using spectro-astrometry. This result also demonstrates for the first time that BD outflows can be collimated and episodic.

  17. The relation between specific baryon angular momentum and mass for a sample of nearby low-mass galaxies with resolved H I kinematics

    Science.gov (United States)

    Elson, E. C.

    2017-12-01

    This paper investigates the relationship between specific baryon angular momentum jb and baryon mass Mb for a sample of nearby late-type galaxies with resolved H I kinematics. This work roughly doubles the number of galaxies with Mb ≲ 1010 M⊙ used to study the jb-Mb relation. Most of the galaxies in the sample have their baryon mass dominated by their gas content, thereby offering jb and Mb measures that are relatively unaffected by uncertainties arising from the stellar mass-to-light ratio. Measured H I surface density radial profiles together with optical and rotation curve data from the literature are used to derive a best-fitting relation given by j_b=qM_b^{α }, with α = 0.62 ± 0.02 and log10 q = -3.35 ± 0.25. This result is consistent with the j_b∝ M_b^{2/3} relation that is theoretically expected and also measured by Obreschkow & Glazebrook for their full sample of THINGS spiral galaxies, yet differs to their steeper relation found for subsets with fixed bulge fraction. The 30 arcsec spatial resolution of the H I imaging used in this study is significantly lower than that of the THINGS imaging used by Obreschkow & Glazebrook, yet the results presented in this work are clearly shown to contain no significant systematic errors due to the low-resolution imaging.

  18. Planck-scale Lorentz violation constrained by ultra-high-energy cosmic rays

    Energy Technology Data Exchange (ETDEWEB)

    Maccione, L. [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany); Univ. Hamburg, II. Inst. fuer Theoretische Physik (Germany); Taylor, A.M. [Max-Planck-Inst. fuer Kernphysik, Heidelberg (Germany); Mattingly, D.M.; Liberati, S. [Scuola Internazionale Superiore di Studi Avanzati SISSA, Trieste (Italy); Istituto Nazionale di Fisica Nucleare INFN, Sezione di Trieste (Italy)

    2009-09-15

    We investigate the consequences of higher dimension Lorentz violating, CPT even kinetic operators that couple standard model fields to a non-zero vector field in an Effective Field Theory framework. Comparing the ultra-high energy cosmic ray spectrum reconstructed in the presence of such terms with data from the Pierre Auger observatory allows us to establish two sided bounds on the coefficients of the mass dimension five and six operators for the proton and pion. Our bounds imply that for both protons and pions, the energy scale of Lorentz symmetry breaking must be well above the Planck scale. In particular, the dimension five operators are constrained at the level of 10{sup -3}M{sup -1}{sub Planck}. The magnitude of the dimension six proton coefficient is bounded at the level of 10{sup -6}M{sup -2}{sub Planck} except in a narrow range where the pion and proton coefficients are both negative and nearly equal. In this small area, the magnitude of the dimension six proton coefficient must only be below 10{sup -3}M{sup -2}{sub Planck}. Constraints on the dimension six pion coefficient are found to be much weaker, but still below M{sup -2}{sub Planck}. (orig.)

  19. Controlled dissolution of silicon dioxide layers for depth resolved multielement analysis by inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Lorge, Susan E.; Houk, R.S.

    2009-01-01

    Dissolution procedures were developed to control the number of surface layers removed, in an attempt to achieve depth resolved analysis by inductively coupled plasma-mass spectrometry (ICP-MS). NIST 612 glass was chosen because it is a homogeneous material with many elements at interesting concentrations, ∼ 50 ppm. Varying dissolution time and HF concentration resulted in the reproducible removal of SiO 2 layers as thin as 70 A deep. Dissolved trace metals were determined after dilution by inductively coupled plasma-mass spectrometry (ICP-MS) with a magnetic sector instrument. The amount removed was determined from the concentration of a major element, Ca. With the exception of Zn, trace metal concentrations agreed reasonably well with their certified values for removal depths of 500, 300 and 150 A. Zinc concentration was significantly high in all dissolutions indicating either a contamination problem or that Zn is removed at a faster rate than Ca. For the dissolutions that removed 70 A of SiO 2 , Cr, Mn, Co, Sr, Cd, Ce, Dy, Er, Yb and U recovery results agreed with their certified values (∼ 50 ppm); Ti, As, Mo, Ba, and Th could not be determined because net intensities were below 3σ of the blank; and measured concentrations for Cu, Pb and Zn were well above the certified values.

  20. Size-resolved mass concentrations of iron oxide aerosols and size-resolved number concentrations of iron oxide aerosols collected from King Air aircraft in Yellow Sea and East China Sea from 2013-02-14 to 2013-03-10 (NCEI Accession 0162201)

    Data.gov (United States)

    National Oceanic and Atmospheric Administration, Department of Commerce — This dataset contains size-resolved mass concentrations of iron oxide aerosols and size-resolved number concentrations of iron oxide aerosols, measured using the...

  1. Flavor characterization of sugar-added pennywort (Centella asiatica L.) juices treated with ultra-high pressure and thermal processes.

    Science.gov (United States)

    Apichartsrangkoon, Arunee; Wongfhun, Pronprapa; Gordon, Michael H

    2009-01-01

    The flavor characteristics of pennywort juices with added sugar treated by ultra-high pressure, pasteurization, and sterilization were investigated using solid phase microextraction combined with gas chromatography-mass spectrometry. It was found that sesquiterpene hydrocarbons comprised the major class of volatile components present and the juices had a characteristic aroma due to the presence of volatiles including beta-caryophyllene and humulene and alpha-copaene. In comparison with heated juices, HPP-treated samples could retain more volatile compounds such as linalool and geraniol similar to those present in fresh juice, whereas some volatiles such as alpha-terpinene and ketone class were apparently formed by thermal treatment. All processing operations produced juice that was not significantly different in the concentration of total volatiles. Practical Application: Pennywort juice is considered a nutraceutical drink for health benefits. Therefore, to preserve all aroma and active components in this juice, a nonthermal process such as ultra-high pressure should be a more appropriate technique for retention of its nutritive values than pasteurization and sterilization.

  2. Imaging Frontostriatal Function in Ultra-High-Risk, Early, and Chronic Schizophrenia During Executive Processing

    Science.gov (United States)

    Morey, Rajendra A.; Inan, Seniha; Mitchell, Teresa V.; Perkins, Diana O.; Lieberman, Jeffrey A.; Belger, Aysenil

    2009-01-01

    Context Individuals experiencing prodromal symptoms of schizophrenia (ultra-high-risk group) demonstrate impaired performance on tasks of executive function, attention, and working memory. The neurobiological underpinnings of such executive deficits in ultra-high-risk individuals remains unclear. Objective We assessed frontal and striatal functions during a visual oddball continuous performance task, in ultra-high-risk, early, and chronic schizophrenic patients with the use of functional magnetic resonance imaging. Design Cross-sectional case-control design. Setting Community; outpatient clinic. Patients Fifty-two individuals (control, n = 16; ultra-high risk, n = 10; early, n = 15; chronic, n = 11) from a referred clinical sample and age- and sex-matched control volunteers underwent scanning. Main Outcome Measures Percentage of active voxels and percentage signal change calculated for the anterior cingulate gyrus (ACG), middle frontal gyrus (MFG), inferior frontal gyrus (IFG), basal ganglia, and thalamus. Performance on the visual oddball task was measured with percentage of hits and d′ (a measure based on the hit rate and the false-alarm rate). Results The ultra-high-risk group showed significantly smaller differential activation between task-relevant and task-irrelevant stimuli in the frontal regions (ACG, IFG, MFG) than the control group. Frontostriatal activation associated with target stimuli in the early and chronic groups was significantly lower than the control group, while the ultra-high-risk group showed a trend toward the early group. Conclusions Our findings suggest that prefrontal function begins to decline before the onset of syndromally defined illness and hence may represent a vulnerability marker in assessing the risk of developing psychotic disorders among ultra-high-risk individuals. PMID:15753238

  3. Ultra-high Efficiency DC-DC Converter using GaN Devices

    DEFF Research Database (Denmark)

    Ramachandran, Rakesh

    2016-01-01

    properties of GaN devices can be utilized in power converters to make them more compact and highly efficient. This thesis entitled “Ultra-high Efficiency DC-DC Converter using GaN devices” focuses on achieving ultra-high conversion efficiency in an isolated dc-dc converter by the optimal utilization of Ga...... for many decades. However, the rate of improvement slowed as the silicon power materials asymptotically approached its theoretical bounds. Compared to Si, wideband gap materials such as Silicon Carbide (SiC) and Gallium Nitride (GaN) are promising semiconductors for power devices due to their superior...... in this thesis. Efficiency measurements from the hardware prototype of both the topologies are also presented in this thesis. Finally, the bidirectional operation of an optimized isolated dc-dc converter is presented. The optimized converter has achieved an ultra-high efficiency of 98.8% in both directions...

  4. Laser beam welding of new ultra-high strength and supra-ductile steels

    Science.gov (United States)

    Dahmen, Martin

    2015-03-01

    Ultra-high strength and supra-ductile are entering fields of new applications. Those materials are excellent candidates for modern light-weight construction and functional integration. As ultra-high strength steels the stainless martensitic grade 1.4034 and the bainitic steel UNS 53835 are investigated. For the supra-ductile steels stand two high austenitic steels with 18 and 28 % manganese. As there are no processing windows an approach from the metallurgical base on is required. Adjusting the weld microstructure the Q+P and the QT steels require weld heat treatment. The HSD steel is weldable without. Due to their applications the ultra-high strength steels are welded in as-rolled and strengthened condition. Also the reaction of the weld on hot stamping is reflected for the martensitic grades. The supra-ductile steels are welded as solution annealed and work hardened by 50%. The results show the general suitability for laser beam welding.

  5. Thermal characterization of Ag and Ag + N ion implanted ultra-high molecular weight polyethylene (UHMWPE)

    Science.gov (United States)

    Sokullu Urkac, E.; Oztarhan, A.; Tihminlioglu, F.; Kaya, N.; Ila, D.; Muntele, C.; Budak, S.; Oks, E.; Nikolaev, A.; Ezdesir, A.; Tek, Z.

    2007-08-01

    Most of total hip joints are composed of ultra-high molecular weight polyethylene (UHMWPE). However, as ultra-high molecular weight polyethylene is too stable in a body, wear debris may accumulate and cause biological response such as bone absorption and loosening of prosthesis. In this study, ultra-high molecular weight polyethylene samples were Ag and Ag + N hybrid ion implanted by using MEVVA ion implantation technique to improve its surface properties. Samples were implanted with a fluence of 1017 ion/cm2 and extraction voltage of 30 kV. Implanted and unimplanted samples were investigated by thermo-gravimetry analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM), optical microscopy (OM) and contact Angle measurement. Thermal characterization results showed that the ion bombardment induced an increase in the % crystallinity, onset and termination degradation temperatures of UHMWPE.

  6. Thermal characterization of Ag and Ag + N ion implanted ultra-high molecular weight polyethylene (UHMWPE)

    Energy Technology Data Exchange (ETDEWEB)

    Sokullu Urkac, E. [Department of Materials Science, Izmir High Technology Institute, Gulbahcekoyu Urla, Izmir (Turkey)]. E-mail: emelsu@gmail.com; Oztarhan, A. [Bioengineering Department, Ege University, Bornova, Izmir 35100 (Turkey); Tihminlioglu, F. [Department of Chemical Engineering, Izmir High Technology Institute, Gulbahcekoyu Urla, Izmir (Turkey); Kaya, N. [Bioengineering Department, Ege University, Bornova, Izmir 35100 (Turkey); Ila, D. [Center for Irradiation of Materials, Alabama A and M University, Normal AL 35762 (United States); Muntele, C. [Center for Irradiation of Materials, Alabama A and M University, Normal AL 35762 (United States); Budak, S. [Center for Irradiation of Materials, Alabama A and M University, Normal AL 35762 (United States); Oks, E. [H C Electronics Institute, Tomsk (Russian Federation); Nikolaev, A. [H C Electronics Institute, Tomsk (Russian Federation); Ezdesir, A. [R and D Department, PETKIM Holding A.S., Aliaga, Izmir 35801 (Turkey); Tek, Z. [Department of Physics, Celal Bayar University, Manisa (Turkey)

    2007-08-15

    Most of total hip joints are composed of ultra-high molecular weight polyethylene (UHMWPE ). However, as ultra-high molecular weight polyethylene is too stable in a body, wear debris may accumulate and cause biological response such as bone absorption and loosening of prosthesis. In this study, ultra-high molecular weight polyethylene samples were Ag and Ag + N hybrid ion implanted by using MEVVA ion implantation technique to improve its surface properties. Samples were implanted with a fluence of 10{sup 17} ion/cm{sup 2} and extraction voltage of 30 kV. Implanted and unimplanted samples were investigated by thermo-gravimetry analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM), optical microscopy (OM) and contact Angle measurement. Thermal characterization results showed that the ion bombardment induced an increase in the % crystallinity, onset and termination degradation temperatures of UHMWPE.

  7. Study on creep of fiber reinforced ultra-high strength concrete based on strength

    Science.gov (United States)

    Peng, Wenjun; Wang, Tao

    2018-04-01

    To complement the creep performance of ultra-high strength concrete, the long creep process of fiber reinforced concrete was studied in this paper. The long-term creep process and regularity of ultra-high strength concrete with 0.5% PVA fiber under the same axial compression were analyzed by using concrete strength (C80/C100/C120) as a variable. The results show that the creep coefficient of ultra-high strength concrete decreases with the increase of concrete strength. Compared with ACI209R (92), GL2000 models, it is found that the predicted value of ACI209R (92) are close to the experimental value, and the creep prediction model suitable for this experiment is proposed based on ACI209R (92).

  8. Design and Implementation of Wideband Exciter for an Ultra-high Resolution Airborne SAR System

    Directory of Open Access Journals (Sweden)

    Jia Ying-xin

    2013-03-01

    Full Text Available According to an ultra-high resolution airborne SAR system with better than 0.1 m resolution, a wideband Linear Frequency Modulated (LFM pulse compression exciter with 14.8 GHz carrier and 3.2 GHz bandwidth is designed and implemented. The selection of signal generation scheme and some key technique points for wideband LFM waveform is presented in detail. Then, an acute test and analysis of the LFM signal is performed. The final airborne experiments demonstrate the validity of the LFM source which is one of the subsystems in an ultra-high resolution airborne SAR system.

  9. All-optical ultra-high-speed OFDM to Nyquist-WDM conversion

    DEFF Research Database (Denmark)

    Guan, Pengyu; Røge, Kasper Meldgaard; Mulvad, Hans Christian Hansen

    2015-01-01

    We propose an all-optical ultra-high-speed OFDM to Nyquist-WDM conversion scheme based on complete OFT. An 8-subcarrier 640 Gbit/s DPSK OFDM super-channel is converted to eight 80-Gbit/s Nyquist-WDM channels with BER <10−9 performance for all channels.......We propose an all-optical ultra-high-speed OFDM to Nyquist-WDM conversion scheme based on complete OFT. An 8-subcarrier 640 Gbit/s DPSK OFDM super-channel is converted to eight 80-Gbit/s Nyquist-WDM channels with BER

  10. Intervention in individuals at ultra-high risk for psychosis: a review and future directions

    DEFF Research Database (Denmark)

    McGorry, Patrick D; Nelson, Barnaby; Amminger, G Paul

    2009-01-01

    OBJECTIVE: Over the last 15 years, a focus on early intervention in psychotic disorders has emerged. Initially, the early psychosis movement focused on timely recognition and phase-specific treatment of first-episode psychosis. However, early psychosis researchers suspected that pushing the point...... of intervention even further back to the prodromal phase of psychotic disorders may result in even better outcomes. This article reviews intervention research in the ultra-high-risk phase of psychotic disorders. DATA SOURCES: A literature search of intervention trials with ultra-high-risk cohorts published after...

  11. Ultra-High-Efficiency Apodized Grating Coupler Using a Fully Etched Photonic Crystal

    DEFF Research Database (Denmark)

    Ding, Yunhong; Peucheret, Christophe; Ou, Haiyan

    2013-01-01

    We demonstrate an apodized fiber-to-chip grating coupler using fully etched photonic crystal holes on the silicon-on-insulator platform. An ultra-high coupling efficiency of 1.65 dB (68%) with 3 dB bandwidth of 60 nm is experimentally demonstrated.......We demonstrate an apodized fiber-to-chip grating coupler using fully etched photonic crystal holes on the silicon-on-insulator platform. An ultra-high coupling efficiency of 1.65 dB (68%) with 3 dB bandwidth of 60 nm is experimentally demonstrated....

  12. A compact Ultra High Vacuum (UHV) compatible instrument for time of flight energy measurements of slow heavy reaction products

    International Nuclear Information System (INIS)

    Kuznetsov, A.V.; Loveland, W.; Jakobsson, B.; Whitlow, H.J.; Bouanani, M. El; Univ. of North Texas, Denton, TX

    2000-01-01

    A compact Ultra High Vacuum (UHV) compatible instrument for time of flight energy measurements of slow heavy reaction products from nuclear reactions has been designed and tested at the CELSIUS storage ring in Uppsala. The construction is based on MicroChannel Plate time detectors of the electron mirror type and silicon p-i-n diodes, and permits the detectors to be stacked side-by-side to achieve large solid angle coverage. This kind of telescope measures the Time of Flight (ToF) and Energy (E) of the particle from which one can reconstruct mass. The combination of an ultra-thin cluster gas-jet target and thin carbon emitter foils allows one to measure heavy residues down to an energy of ∼ 35 keV/nucleon from the interactions of 400 MeV/nucleon 16 O with nat Xe gas targets

  13. A compact Ultra High Vacuum (UHV) compatible instrument for time of flight energy measurements of slow heavy reaction products

    Energy Technology Data Exchange (ETDEWEB)

    Kuznetsov, A.V. [V.G.Khlopin Radium Institute, St. Petersburg (Russian Federation); Uppsala Univ. (Sweden). The Svedberg Lab.; Veldhuizen, E.J. van; Aleklett, K. [Uppsala Univ., (Sweden). Dept. of Radiation Sciences; Westerberg, L. [Uppsala University (Sweden). The Svedberg Lab.; Lyapin, V.G. [V.G.Khlopin Radium Institute, St. Petersburg (Russian Federation); Loveland, W. [Oregon State Univ., Corvallis, OR (United States). Dept. of Chemistry; Bondorf, J. [Niels Bohr Inst., Copenhagen (Denmark); Jakobsson, B. [Lund Univ. (Sweden). Dept. of Physics; Whitlow, H.J. [Lund Univ. (Sweden). Dept. of Nuclear Physics; Bouanani, M. El [Lund Univ. (Sweden). Dept. of Nuclear Physics; Univ. of North Texas, Denton, TX (United States). Dept. of Physics

    2000-07-01

    A compact Ultra High Vacuum (UHV) compatible instrument for time of flight energy measurements of slow heavy reaction products from nuclear reactions has been designed and tested at the CELSIUS storage ring in Uppsala. The construction is based on MicroChannel Plate time detectors of the electron mirror type and silicon p-i-n diodes, and permits the detectors to be stacked side-by-side to achieve large solid angle coverage. This kind of telescope measures the Time of Flight (ToF) and Energy (E) of the particle from which one can reconstruct mass. The combination of an ultra-thin cluster gas-jet target and thin carbon emitter foils allows one to measure heavy residues down to an energy of {approx} 35 keV/nucleon from the interactions of 400 MeV/nucleon {sup 16}O with {sup nat} Xe gas targets.

  14. Bioactivity evaluation-based ultra high-performance liquid chromatography coupled with electrospray ionization tandem quadrupole-time-of-flight mass spectrometry and novel distinction of multi-subchemome compatibility recognition strategy with Astragali Radix-Fructus Corni herb-pair as a case study.

    Science.gov (United States)

    Duan, Yu; Pei, Ke; Cai, Hao; Tu, Sicong; Zhang, Zhengwei; Cheng, Xinwei; Qiao, Fengxian; Fan, Kailei; Qin, Kunming; Liu, Xiao; Cai, Baochang

    2016-09-10

    The approach to investigate traditional Chinese medicine (TCM) is still in its infancy and has been facing enormous challenge. In this paper, a generally applicable strategy was developed for investigation on TCM systematically with an introduced interesting idea about a novel research system which called subchemome. A representative herb-pair, Astragali Radix-Fructus Corni, was successfully employed to expound this novel strategy. Firstly, subchemomes were prepared individually by applying the suitable column chromatography, each of them was detected by UV spectrophotometer or HPLC-DAD detector. The components in each part were then identified based on the mass spectrometric fragmentation patterns and tandem mass spectrometric data by using UHPLC-Q-TOF-MS. Using renal mesangial cell (RMC) viability assay as the evaluation of the pharmacological activity of each group, we developed the new mini herbal formulae aimed at diabetic nephropathy and identified fifteen marker components between the group of new mini herbal formulae and other groups from the angle of the constituent, and then explored the effects of new mini herbal formulae from another angle of the molecular mechanism. Overall, the presently developed strategy should be beneficial and widely used in the investigation on TCM from a new perspective. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Ultra-High Resolution Spectroscopic Remote Sensing: A Microscope on Planetary Atmospheres

    Science.gov (United States)

    Kostiuk, Theodor

    2010-01-01

    Remote sensing of planetary atmospheres is not complete without studies of all levels of the atmosphere, including the dense cloudy- and haze filled troposphere, relatively clear and important stratosphere and the upper atmosphere, which are the first levels to experience the effects of solar radiation. High-resolution spectroscopy can provide valuable information on these regions of the atmosphere. Ultra-high spectral resolution studies can directly measure atmospheric winds, composition, temperature and non-thermal phenomena, which describe the physics and chemistry of the atmosphere. Spectroscopy in the middle to long infrared wavelengths can also probe levels where dust of haze limit measurements at shorter wavelength or can provide ambiguous results on atmospheric species abundances or winds. A spectroscopic technique in the middle infrared wavelengths analogous to a radio receiver. infrared heterodyne spectroscopy [1], will be describe and used to illustrate the detailed study of atmospheric phenomena not readily possible with other methods. The heterodyne spectral resolution with resolving power greater than 1,000.000 measures the true line shapes of emission and absorption lines in planetary atmospheres. The information on the region of line formation is contained in the line shapes. The absolute frequency of the lines can be measured to I part in 100 ,000,000 and can be used to accurately measure the Doppler frequency shift of the lines, directly measuring the line-of-sight velocity of the gas to --Im/s precision (winds). The technical and analytical methods developed and used to measure and analyze infrared heterodyne measurements will be described. Examples of studies on Titan, Venus, Mars, Earth, and Jupiter will be presented. 'These include atmospheric dynamics on slowly rotating bodies (Titan [2] and Venus [3] and temperature, composition and chemistry on Mars 141, Venus and Earth. The discovery and studies of unique atmospheric phenomena will also be

  16. CHEOPS: a space telescope for ultra-high precision photometry of exoplanet transits

    Science.gov (United States)

    Cessa, V.; Beck, T.; Benz, W.; Broeg, C.; Ehrenreich, D.; Fortier, A.; Peter, G.; Magrin, D.; Pagano, I.; Plesseria, J.-Y.; Steller, M.; Szoke, J.; Thomas, N.; Ragazzoni, R.; Wildi, F.

    2017-11-01

    The CHaracterising ExOPlanet Satellite (CHEOPS) is a joint ESA-Switzerland space mission dedicated to search for exoplanet transits by means of ultra-high precision photometry whose launch readiness is expected end 2017. The CHEOPS instrument will be the first space telescope dedicated to search for transits on bright stars already known to host planets. By being able to point at nearly any location on the sky, it will provide the unique capability of determining accurate radii for a subset of those planets for which the mass has already been estimated from ground-based spectroscopic surveys. CHEOPS will also provide precision radii for new planets discovered by the next generation ground-based transits surveys (Neptune-size and smaller). The main science goals of the CHEOPS mission will be to study the structure of exoplanets with radii typically ranging from 1 to 6 Earth radii orbiting bright stars. With an accurate knowledge of masses and radii for an unprecedented sample of planets, CHEOPS will set new constraints on the structure and hence on the formation and evolution of planets in this mass range. To reach its goals CHEOPS will measure photometric signals with a precision of 20 ppm in 6 hours of integration time for a 9th magnitude star. This corresponds to a signal to noise of 5 for a transit of an Earth-sized planet orbiting a solar-sized star (0.9 solar radii). This precision will be achieved by using a single frame-transfer backside illuminated CCD detector cool down at 233K and stabilized within {10 mK . The CHEOPS optical design is based on a Ritchey-Chretien style telescope with 300 mm effective aperture diameter, which provides a defocussed image of the target star while minimizing straylight using a dedicated field stop and baffle system. As CHEOPS will be in a LEO orbit, straylight suppression is a key point to allow the observation of faint stars. The telescope will be the only payload on a spacecraft platform providing pointing stability of

  17. Ultra-High-Performance Concrete And Advanced Manufacturing Methods For Modular Construction

    Energy Technology Data Exchange (ETDEWEB)

    Sawab, Jamshaid [Univ. of Houston, Houston, TX (United States); Lim, Ing [Univ. of Houston, Houston, TX (United States); Mo, Yi-Lung [Univ. of Houston, Houston, TX (United States); Li, Mo [Univ. of Houston, Houston, TX (United States); Wang, Hong [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Guimaraes, Maria [Electric Power Research Inst. (EPRI), Knoxville, TN (United States)

    2016-04-13

    Small modular reactors (SMR) allow for less onsite construction, increase nuclear material security, and provide a flexible and cost-effective energy alternative. SMR can be factory-built as modular components, and shipped to desired locations for fast assembly. This project successfully developed a new class of ultra-high performance concrete (UHPC), which features a compressive strength greater than 22 ksi (150 MPa) without special treatment and self-consolidating characteristics desired for SMR modular construction. With an ultra-high strength and dense microstructure, it will facilitate rapid construction of steel plate-concrete (SC) beams and walls with thinner and lighter modules, and can withstand harsh environments and mechanical loads anticipated during the service life of nuclear power plants. In addition, the self-consolidating characteristics are crucial for the fast construction and assembly of SC modules with reduced labor costs and improved quality. Following the UHPC material development, the capacity of producing self-consolidating UHPC in mass quantities was investigated and compared to accepted self-consolidating concrete standards. With slightly adjusted mixing procedure using large-scale gravity-based mixers (compared with small-scale force-based mixer), the self-consolidating UHPC has been successfully processed at six cubic yards; the product met both minimum compressive strength requirements and self-consolidating concrete standards. Steel plate-UHPC beams (15 ft. long, 12 in. wide and 16 in. deep) and wall panels (40 in. X 40 in. X 3 in.) were then constructed using the self-consolidating UHPC without any external vibration. Quality control guidelines for producing UHPC in large scale were developed. When the concrete is replaced by UHPC in a steel plate concrete (SC) beam, it is critical to evaluate its structural behavior with both flexure and shear-governed failure modes. In recent years, SC has been widely used for buildings and nuclear

  18. Propagation of ultra-high-energy cosmic rays and their secondaries with CRPropa

    International Nuclear Information System (INIS)

    Vliet, Arjen Rene van

    2015-04-01

    Due to experiments like the Pierre Auger Observatory (Auger) and the Telescope Array (TA), high-statistics data is becoming available on the energy spectrum, the composition and the arrival directions of ultra-high-energy cosmic rays (UHECRs, cosmic rays with energies above ∝ 10 17 eV). To interpret this data in terms of actual astrophysical parameters, or to test astrophysical models against the measured data, dedicated simulations of the propagation of UHECRs from their sources to Earth are needed. To this end, the UHECR propagation code called CRPropa has been developed. It can take into account all relevant interactions with ambient photon backgrounds (pair production, photodisintegration and photopion production) as well as nuclear decay, cosmological evolution effects and deflections in extragalactic and galactic magnetic fields. CRPropa, including its newest features, is described in this thesis. When considering the propagation of ultra-high-energy nuclei, the dominant interaction for most isotopes and energies is photodisintegration. Photodisintegration has been implemented in CRPropa for all relevant isotopes (up to iron) and all relevant photodisintegration channels using cross-section calculations with the publicly-available code called TALYS, including extensions for the low mass numbers. This photodisintegration setup is compared here extensively with the photodisintegration scheme developed by Puget, Stecker and Bredekamp, leading to several improvements on the cross sections implemented in CRPropa. In the interactions of UHECRs with background photon fields, secondary neutrinos and photons, so-called cosmogenic neutrinos and photons, can be created. CRPropa can simulate the production and propagation of these secondary particles as well. The IceCube Neutrino Observatory (IceCube) has recently reported the first observation of extraterrestrial neutrinos in the PeV energy range. In this work is investigated whether these neutrinos could have

  19. [Reparative Osteogenesis and Angiogenesis in Low Intensity Electromagnetic Radiation of Ultra-High Frequency].

    Science.gov (United States)

    Iryanov, Y M; Kiryanov, N A

    2015-01-01

    Non-drug correction of reparative bone tissue regeneration in different pathological states - one of the most actual problems of modern medicine. Our aim was to conduct morphological analysis of the influence of electromagnetic radiation of ultra-high frequency and low intensity on reparative osteogenesis and angiogenesis in fracture treatment under transosseous osteosynthesis. A controlled nonrandomized study was carried out. In the experiment conducted on rats we modeled tibial fracture with reposition and fixation of the bone fragments both in control and experimental groups. In the animals of the experimental group the fracture zone was exposed to low intensity electromagnetic radiation of ultra-high frequency. Exposure simulation was performed in the control group. The operated bones were examined using radiography, light and electronic microscopy, X-ray electronic probe microanalysis. It has been established that electromagnetic radiation of ultra-high frequency sessions in fracture treatment stimulate secretory activity and degranulation of mast cells, produce microcirculatory bed vascular permeability increase, endotheliocyte migration phenotype expression, provide endovascular endothelial outgrowth formation, activate reparative osteogenesis and angiogenesis while fracture reparation becomes the one of the primary type. The full periosteal, intermediary and intraosteal bone union was defined in 28 days. Among the therapeutic benefits of electromagnetic radiation of ultra-high frequency in fracture treatment we can detect mast cell secretorv activity stimulation and endovascular anziozenesis activation.

  20. Bond behavior of reinforcing steel in ultra-high performance concrete.

    Science.gov (United States)

    2014-10-01

    Ultra-High Performance Concrete (UHPC) is a relatively new class of advanced cementitious composite : materials, which exhibits high compressive [above 21.7 ksi (150 MPa)] and tensile [above 0.72 ksi (5 MPa)] : strengths. The discrete steel fiber rei...

  1. Case study: dairies utilizing ultra-high stocking density grazing in Pennsylvania and New York

    Science.gov (United States)

    Ultra-high stocking density (UHSD) grazing has gained interest in the forage industry. Proponents of UHSD emphasize increased forage use efficiency and soil improvement by grazing mature forage with stocking densities up to 560,425 kg ha**-1 of beef cattle on small paddocks with rest periods of up t...

  2. Ultra-high aspect ratio replaceable AFM tips using deformation-suppressed focused ion beam milling

    DEFF Research Database (Denmark)

    Savenko, Alexey; Yildiz, Izzet; Petersen, Dirch Hjorth

    2013-01-01

    Fabrication of ultra-high aspect ratio exchangeable and customizable tips for atomic force microscopy (AFM) using lateral focused ion beam (FIB) milling is presented. While on-axis FIB milling does allow high aspect ratio (HAR) AFM tips to be defined, lateral milling gives far better flexibility...

  3. Solutions for ultra-high speed optical wavelength conversion and clock recovery

    DEFF Research Database (Denmark)

    Oxenløwe, Leif Katsuo; Galili, Michael; Mulvad, Hans Christian Hansen

    2006-01-01

    This paper reports on our recent advances in ultra-fast optical communications relying on ultra-short pulses densely stacked in ultra-high bit rate serial data signals at a single wavelength. The paper describes details in solutions for the network functionalities of wavelength conversion and clock...... recovery at bit rates up to 320 Gb/s...

  4. Social cognition in patients at ultra-high risk for psychosis

    DEFF Research Database (Denmark)

    Glenthøj, Louise B.; Fagerlund, Birgitte; Hjorthøj, Carsten

    2016-01-01

    Objective: Patients at ultra-high risk (UHR) for psychosis show significant impairments in functioning. It is essential to determine which factors influence functioning, as it may have implications for intervention strategies. This study examined whether social cognitive abilities and clinical...

  5. Overview of lunar detection of ultra-high energy particles and new plans for the SKA

    NARCIS (Netherlands)

    James, Clancy W.; Alvarez-Muñiz, Jaime; Bray, Justin D.; Buitink, Stijn; Dagkesamanskii, Rustam D.; Ekers, Ronald D.; Falcke, Heino; Gayley, Ken; Huege, Tim; Mevius, Maaijke; Mutel, Rob; Scholten, Olaf; Spencer, Ralph; ter Veen, Sander; Winchen, Tobias

    2017-01-01

    The lunar technique is a method for maximising the collection area for ultra-high-energy (UHE) cosmic ray and neutrino searches. The method uses either ground-based radio telescopes or lunar orbiters to search for Askaryan emission from particles cascading near the lunar surface. While experiments

  6. Ultra-high efficiency, fast graphene micro-heater on silicon

    DEFF Research Database (Denmark)

    Yan, Siqi; Zhu, Xiaolong; Frandsen, Lars Hagedorn

    2017-01-01

    We demonstrate an ultra-high efficiency and fast graphene microheater on silicon photonic crystal waveguide. By taking advantage of slow-light effect, a tuning efficiency of 1.07 nm/mW and power consumption per free spectral range of 3.99 mW. A fast rise and decay times (10% to 90%) of only 750 ns...

  7. The adhesive properties of chlorinated ultra-high molecular weight polyethylene

    NARCIS (Netherlands)

    Menting, H.N.A.M.; Voets, P.E.L.; Lemstra, P.J.

    1995-01-01

    Ultra-high molecular weight polyethylene (UHMW-PE) is well known for its abrasion and chemical resistance. Recently we developed a new application for UHMW-PE as a liner in elastomeric hoses. It was found that the adhesion between UHMW-PE and elastomers such as ethylene-propylene-diene monomer

  8. Extension induced phase separation and crystallization in semidilute solutions of ultra high molecular weight polyethylene

    DEFF Research Database (Denmark)

    Wingstrand, Sara Lindeblad; Imperiali, Luna; Stepanyan, Roman

    2018-01-01

    Abstract We investigate the influence of controlled uniaxial extension on various flow induced phenomena in semidilute solutions of ultra high molecular weight polyethylene (UHMwPE). Concentrations range from 9 w% to 29 w% and the choice of solvent is paraffin oil (PO). The start-up extensional b...

  9. OTR profile measurement of a LINAC electron beam with portable ultra high-speed camera

    International Nuclear Information System (INIS)

    Mogi, T.; Nisiyama, S.; Tomioka, S.; Enoto, T.

    2004-01-01

    We have studied on and developed a portable ultra high-speed camera, and so applied to measurement of a LINAC electron beam. We measured spatial OTR profiles of a LINAC electron beam using this camera with temporal resolution 80ns. (author)

  10. 78 FR 70567 - Nationwide Use of High Frequency and Ultra High Frequency Active SONAR Technology; Final...

    Science.gov (United States)

    2013-11-26

    ... Frequency and Ultra High Frequency Active SONAR Technology; Final Programmatic Environmental Assessment and... each alternative on the human and natural environments. FOR FURTHER INFORMATION CONTACT: If you have... Programmatic Environmental Assessment The scope of the PEA focuses on potential impacts associated with the...

  11. Nanometer size wear debris generated from ultra high molecular weight polyethylene in vivo

    Czech Academy of Sciences Publication Activity Database

    Lapčíková, Monika; Šlouf, Miroslav; Dybal, Jiří; Zolotarevova, E.; Entlicher, G.; Pokorný, D.; Gallo, J.; Sosna, A.

    2009-01-01

    Roč. 266, 1-2 (2009), s. 349-355 ISSN 0043-1648 R&D Projects: GA MŠk 2B06096 Institutional research plan: CEZ:AV0Z40500505 Keywords : ultra high molecular weight polyethylene * nanometer size wear debris * morphology of wear particles Subject RIV: CD - Macromolecular Chemistry Impact factor: 1.771, year: 2009

  12. Detection of ultra-high energy cosmic ray showers with a single-pixel fluorescence telescope

    Czech Academy of Sciences Publication Activity Database

    Fujii, T.; Malacari, M.; Bertaina, M.; Casolino, E.; Dawson, B.; Horváth, P.; Hrabovský, M.; Jiang, J.; Mandát, Dušan; Matalon, A.; Matthews, J.N.; Motloch, P.; Palatka, Miroslav; Pech, Miroslav; Privitera, P.; Schovánek, Petr; Takizawa, Y.; Thomas, S.B.; Trávníček, Petr; Yamazaki, K.

    2016-01-01

    Roč. 74, Feb (2016), s. 64-72 ISSN 0927-6505 R&D Projects: GA MŠk(CZ) LG13007 Institutional support: RVO:68378271 Keywords : ultra-high energy cosmic rays * fluorescence detector * extensive air shower Subject RIV: BF - Elementary Particles and High Energy Physics Impact factor: 3.257, year: 2016

  13. The MIDAS telescope for microwave detection of ultra-high energy cosmic rays

    Czech Academy of Sciences Publication Activity Database

    Alvarez-Muñiz, J.; Soares, E.A.; Berlin, A.; Bogdan, M.; Boháčová, Martina; Bonifazi, C.; Carvalho, W.R.; de Mello Neto, J.R.T.; San Luis, P.F.; Genat, J.F.; Hollon, N.; Mills, E.; Monasor, M.; Privitera, P.; Ramos de Castro, A.; Reyes, L.C.; Richardson, M.; Rouille D’Orfeuil, B.; Santos, E.M.; Wayne, S.; Williams, C.; Zas, E.; Zhou, J.

    2013-01-01

    Roč. 719, Aug (2013), s. 70-80 ISSN 0168-9002 Institutional support: RVO:68378271 Keywords : ultra high energy cosmic rays * radio-detection * microwave * GHz Subject RIV: BF - Elementary Particles and High Energy Physics Impact factor: 1.316, year: 2013

  14. Deformation and degradation of polymers in ultra-high-pressure liquid chromatography

    NARCIS (Netherlands)

    Uliyanchenko, E.; van der Wal, S.; Schoenmakers, P.J.

    2011-01-01

    Ultra-high-pressure liquid chromatography (UHPLC) using columns packed with sub-2 μm particles has great potential for separations of many types of complex samples, including polymers. However, the application of UHPLC for the analysis of polymers meets some fundamental obstacles. Small particles

  15. Fornax A, Centaurus A other radio galaxies as sources of ultra-high energy cosmic rays

    Science.gov (United States)

    Matthews, J. H.; Bell, A. R.; Blundell, K. M.; Araudo, A. T.

    2018-06-01

    The origin of ultra-high energy cosmic rays (UHECRs) is still unknown. It has recently been proposed that UHECR anisotropies can be attributed to starburst galaxies or active galactic nuclei. We suggest that the latter is more likely and that giant-lobed radio galaxies such as Centaurus A and Fornax A can explain the data.

  16. Kinetic and thermodynamic analysis of ultra-high pressure and heat ...

    African Journals Online (AJOL)

    Purpose: To undertake comparative kinetic and thermodynamic analyses of the interaction of bovine serum albumin (BSA) with IgG pre-treated with ultra-high pressure (UHP) and moderate heat. Methods: BSA solutions were processed at 100 – 600 MPa and 25 – 40 °C. We applied an optical biosensor based on surface ...

  17. Adaptive sensor-based ultra-high accuracy solar concentrator tracker

    Science.gov (United States)

    Brinkley, Jordyn; Hassanzadeh, Ali

    2017-09-01

    Conventional solar trackers use information of the sun's position, either by direct sensing or by GPS. Our method uses the shading of the receiver. This, coupled with nonimaging optics design allows us to achieve ultra-high concentration. Incorporating a sensor based shadow tracking method with a two stage concentration solar hybrid parabolic trough allows the system to maintain high concentration with acute accuracy.

  18. The Heart of China revisited: II Early Paleozoic (ultra)high-pressure and (ultra)high-temperature metamorphic Qinling orogenic collage

    Science.gov (United States)

    Bader, Thomas; Franz, Leander; Ratschbacher, Lothar; de Capitani, Christian; Webb, A. Alexander G.; Yang, Zhao; Pfänder, Jörg A.; Hofmann, Mandy; Linnemann, Ulf

    2013-07-01

    Orogens with multiple (ultra)high-pressure ((U)HP) and (ultra)high-temperature ((U)HT) metamorphic events provide a complex but telling record of oceanic and continental interaction. The Early Paleozoic history of the "Heart of China," the Qinling orogenic collage, offers snapshots of at least three (U)HP and two (U)HT metamorphic events. The preservation of remnants of both oceanic and continental domains together with a ≥110 Myr record of magmatism allows the reconstruction of the processes that resulted in this disparate metamorphism. Herein, we first illuminate the pressure-temperature-time (P-T-t) evolution of the Early Paleozoic (U)HP and (U)HT events by refining the petrographic descriptions and P-T estimates, assess published, and employ new U/Th-Pb zircon, monazite, and titanite, and 40Ar-39Ar phengite geochronology to date the magmatic and metamorphic events. Then we explore how the metamorphic and magmatic events are related tectonically and how they elucidate the affinities among the various complexes in the Qinling orogenic collage. We argue that a Meso-Neoproterozoic crustal fragment—the Qinling complex—localized subduction-accretion events that involved subduction, oceanic-arc formation, and back-arc spreading along its northern margin, and mtantle-wedge exhumation and spreading-ridge subduction along its southern margin.

  19. Industry-relevant magnetron sputtering and cathodic arc ultra-high vacuum deposition system for in situ x-ray diffraction studies of thin film growth using high energy synchrotron radiation

    OpenAIRE

    Schroeder, Jeremy; Thomson, W.; Howard, B.; Schell, N.; Näslund, Lars-Åke; Rogström, Lina; Johansson-Jöesaar, Mats P.; Ghafoor, Naureen; Odén, Magnus; Nothnagel, E.; Shepard, A.; Greer, J.; Birch, Jens

    2015-01-01

    We present an industry-relevant, large-scale, ultra-high vacuum (UHV) magnetron sputtering and cathodic arc deposition system purposefully designed for time-resolved in situ thin film deposition/annealing studies using high-energy (greater than50 keV), high photon flux (greater than10(12) ph/s) synchrotron radiation. The high photon flux, combined with a fast-acquisition-time (less than1 s) two-dimensional (2D) detector, permits time-resolved in situ structural analysis of thin film formation...

  20. Ultra high-speed x-ray imaging of laser-driven shock compression using synchrotron light

    Science.gov (United States)

    Olbinado, Margie P.; Cantelli, Valentina; Mathon, Olivier; Pascarelli, Sakura; Grenzer, Joerg; Pelka, Alexander; Roedel, Melanie; Prencipe, Irene; Laso Garcia, Alejandro; Helbig, Uwe; Kraus, Dominik; Schramm, Ulrich; Cowan, Tom; Scheel, Mario; Pradel, Pierre; De Resseguier, Thibaut; Rack, Alexander

    2018-02-01

    A high-power, nanosecond pulsed laser impacting the surface of a material can generate an ablation plasma that drives a shock wave into it; while in situ x-ray imaging can provide a time-resolved probe of the shock-induced material behaviour on macroscopic length scales. Here, we report on an investigation into laser-driven shock compression of a polyurethane foam and a graphite rod by means of single-pulse synchrotron x-ray phase-contrast imaging with MHz frame rate. A 6 J, 10 ns pulsed laser was used to generate shock compression. Physical processes governing the laser-induced dynamic response such as elastic compression, compaction, pore collapse, fracture, and fragmentation have been imaged; and the advantage of exploiting the partial spatial coherence of a synchrotron source for studying low-density, carbon-based materials is emphasized. The successful combination of a high-energy laser and ultra high-speed x-ray imaging using synchrotron light demonstrates the potentiality of accessing complementary information from scientific studies of laser-driven shock compression.

  1. Measurement of the ultra high energy cosmic ray flux from data of very inclined showers at the Pierre Auger Observatory

    International Nuclear Information System (INIS)

    Dembinski, Hans Peter

    2009-01-01

    This work describes the derivation of the energy dependent flux of ultra-high energy cosmic rays from data of very inclined air showers observed with the Pierre Auger Observatory. It focuses on the event class of very inclined air showers with zenith angles larger than 60 . The lateral ground profile of these showers is muon dominated and not radially symmetric around the shower axis due to geomagnetic deflections and other effects. The dependency of this profile on the direction, energy and mass of the cosmic ray is discussed with a mixture of detailed Monte-Carlo simulations and a simplified analytical model of the air shower cascade. It is found in agreement with other studies that the normalized shape of the muon density profile is approximately universal over the range of cosmic ray energies and masses measured at the Pierre Auger Observatory, that the amplitude of the profile is almost proportional to the cosmic ray energy, and that its shower-to-shower fluctuations are sensitive to the mass composition of the cosmic rays. (orig.)

  2. Measurement of the ultra high energy cosmic ray flux from data of very inclined showers at the Pierre Auger Observatory

    Energy Technology Data Exchange (ETDEWEB)

    Dembinski, Hans Peter

    2009-12-03

    This work describes the derivation of the energy dependent flux of ultra-high energy cosmic rays from data of very inclined air showers observed with the Pierre Auger Observatory. It focuses on the event class of very inclined air showers with zenith angles larger than 60 . The lateral ground profile of these showers is muon dominated and not radially symmetric around the shower axis due to geomagnetic deflections and other effects. The dependency of this profile on the direction, energy and mass of the cosmic ray is discussed with a mixture of detailed Monte-Carlo simulations and a simplified analytical model of the air shower cascade. It is found in agreement with other studies that the normalized shape of the muon density profile is approximately universal over the range of cosmic ray energies and masses measured at the Pierre Auger Observatory, that the amplitude of the profile is almost proportional to the cosmic ray energy, and that its shower-to-shower fluctuations are sensitive to the mass composition of the cosmic rays. (orig.)

  3. Enhancing ultra-high CPV passive cooling using least-material finned heat sinks

    Energy Technology Data Exchange (ETDEWEB)

    Micheli, Leonardo, E-mail: lm409@exeter.ac.uk; Mallick, Tapas K., E-mail: T.K.Mallick@exeter.ac.uk [Environment and Sustainability Institute, University of Exeter, Penryn, Cornwall TR10 9FE (United Kingdom); Fernandez, Eduardo F., E-mail: E.Fernandez-Fernandez2@exeter.ac.uk [Environment and Sustainability Institute, University of Exeter, Penryn, Cornwall TR10 9FE (United Kingdom); Centre of Advanced Studies in Energy and Environment, University of Jaen, Jaen 23071 (Spain); Almonacid, Florencia, E-mail: facruz@ujaen.es [Centre of Advanced Studies in Energy and Environment, University of Jaen, Jaen 23071 (Spain); Reddy, K. S., E-mail: ksreddy@iitm.ac.in [Department of Mechanical Engineering, Indian Institute of Technology Madras, Chennai, 600036 (India)

    2015-09-28

    Ultra-high concentrating photovoltaic (CPV) systems aim to increase the cost-competiveness of CPV by increasing the concentrations over 2000 suns. In this work, the design of a heat sink for ultra-high concentrating photovoltaic (CPV) applications is presented. For the first time, the least-material approach, widely used in electronics to maximize the thermal dissipation while minimizing the weight of the heat sink, has been applied in CPV. This method has the potential to further decrease the cost of this technology and to keep the multijunction cell within the operative temperature range. The designing procedure is described in the paper and the results of a thermal simulation are shown to prove the reliability of the solution. A prediction of the costs is also reported: a cost of 0.151$/W{sub p} is expected for a passive least-material heat sink developed for 4000x applications.

  4. Study of application technology of ultra-high speed computer to the elucidation of complex phenomena

    International Nuclear Information System (INIS)

    Sekiguchi, Tomotsugu

    1996-01-01

    The basic design of numerical information library in the decentralized computer network was explained at the first step of constructing the application technology of ultra-high speed computer to the elucidation of complex phenomena. Establishment of the system makes possible to construct the efficient application environment of ultra-high speed computer system to be scalable with the different computing systems. We named the system Ninf (Network Information Library for High Performance Computing). The summary of application technology of library was described as follows: the application technology of library under the distributed environment, numeric constants, retrieval of value, library of special functions, computing library, Ninf library interface, Ninf remote library and registration. By the system, user is able to use the program concentrating the analyzing technology of numerical value with high precision, reliability and speed. (S.Y.)

  5. The Promise and Challenges of Ultra High Bypass Ratio Engine Technology and Integration

    Science.gov (United States)

    Hughes, Chris

    2011-01-01

    In this presentation, an overview of the research being conducted by the ERA Project in Ultra High Bypass aircraft propulsion and in partnership with Pratt & Whitney with their Geared TurboFan (GTF) is given. The ERA goals are shown followed by a discussion of what areas need to be addressed on the engine to achieve the goals and how the GTF is uniquely qualified to meet the goals through a discussion of what benefits the cycle provides. The first generation GTF architecture is then shown highlighting the areas of collaboration with NASA, and the fuel burn, noise and emissions reductions possible based on initial static ground test and flight test data of the first GTF engine. Finally, a 5 year technology roadmap is presented focusing on Ultra High Bypass propulsion technology research areas that are being pursued and being planned by ERA and P&W under their GTF program.

  6. Ultra-high density aligned Carbon-nanotube with controled nano-morphology for supercapacitors

    Science.gov (United States)

    Ghaffari, Mehdi; Zhao, Ran; Liu, Yang; Zhou, Yue; Cheng, Jiping; Guzman de Villoria, Roberto; Wardle, B. L.; Zhang, Q. M.

    2012-02-01

    Recent advances in fabricating controlled-morphology vertically aligned carbon nanotubes (VA-CNTs) with ultrahigh volume fractioncreate unique opportunities for developing unconventional supercapacitors with ultra-high energy density, power density, and long charge/discharge cycle life.Continuous paths through inter-VA-CNT channels allow fast ion transport, and high electrical conduction of the aligned CNTs in the composite electrodes lead to fast discharge speed. We investigate the charge-discharge characteristics of VA-CNTs with >20 vol% of CNT and ionic liquids as electrolytes. By employing both the electric and electromechanical spectroscopes, as well as nanostructured materials characterization, the ion transport and storage behaviors in porous electrodes are studied. The results suggest pathways for optimizing the electrode morphology in supercapacitorsusing ultra-high volume fraction VA-CNTs to further enhance performance.

  7. Processing and evaluation of the AGS Booster ultra-high vaccum system

    International Nuclear Information System (INIS)

    Hseuh, H.C.; Mapes, M.; Schnitzenbaumer, P.; Shen, B.; Sikora, R.; Stattel, P.

    1991-01-01

    The AGS Booster is a synchrotron for the acceleration of both protons and heavy ions. To minimize the beam loss due to charge exchange of the partially stripped, low Β very heavy ions with the residual gas molecules, pressure of low 10 -11 Torr is required for the 200 m booster ring. To achieve this ultra high vacuum, chemical cleaning, vacuum furnace degassing and insitu bake were employed for all chambers and beam components. Using these procedures, vacuums of low 10 -11 Torr have been routinely achieved during the testing of individual half cells and beam components, and during the commissioning of the vacuum sectors. In this paper, the design and layout of chambers, flanges and bakeout hardware is briefly described. The vacuum processing of different components and the results of bakeout and evaluation are summarized. The experience gained during the construction and commissioning of this ultra-high vacuum system is also given. 3 refs., 3 figs., 1 tab

  8. Cavity resonance absorption in ultra-high bandwidth CRT deflection structure by a resistive load

    Science.gov (United States)

    Dunham, M.E.; Hudson, C.L.

    1993-05-11

    An improved ultra-high bandwidth helical coil deflection structure for a cathode ray tube is described comprising a first metal member having a bore therein, the metal walls of which form a first ground plane; a second metal member coaxially mounted in the bore of the first metal member and forming a second ground plane; a helical deflection coil coaxially mounted within the bore between the two ground planes; and a resistive load disposed in one end of the bore and electrically connected to the first and second ground planes, the resistive load having an impedance substantially equal to the characteristic impedance of the coaxial line formed by the two coaxial ground planes to inhibit cavity resonance in the structure within the ultra-high bandwidth of operation. Preferably, the resistive load comprises a carbon film on a surface of an end plug in one end of the bore.

  9. Ultra-high temperature tensile properties of ODS steel claddings under severe accident conditions

    Energy Technology Data Exchange (ETDEWEB)

    Yano, Y., E-mail: yano.yasuhide@jaea.go.jp [Japan Atomic Energy Agency, 4002, Narita-cho, Oarai-machi, Ibaraki, 311-1393 (Japan); Tanno, T.; Oka, H.; Ohtsuka, S.; Inoue, T.; Kato, S.; Furukawa, T.; Uwaba, T.; Kaito, T. [Japan Atomic Energy Agency, 4002, Narita-cho, Oarai-machi, Ibaraki, 311-1393 (Japan); Ukai, S.; Oono, N. [Materials Science and Engineering, Faculty of Engineering, Hokkaido University, N13, W-8, Kita-ku, Sapporo, Hokkaido, 060-8628 (Japan); Kimura, A. [Institute of Advanced Energy, Kyoto University, Gokasho, Uji, Kyoto 611-0011 (Japan); Hayashi, S. [Tokyo Institute of Technology, 2-12-1, Ookayama, Meguro-ku, Tokyo 152-8550 (Japan); Torimaru, T. [Nippon Nuclear Fuel Development Co., Ltd., 2163, Narita-cho, Oarai-machi, Ibaraki, 311-1313 (Japan)

    2017-04-15

    Ultra-high temperature ring tensile tests were performed to investigate the tensile behavior of oxide dispersion strengthened (ODS) steel claddings and wrapper materials under severe accident conditions with temperatures ranging from room temperature to 1400 °C which is close to the melting point of core materials. The experimental results showed that the tensile strength of 9Cr-ODS steel claddings was highest in the core materials at ultra-high temperatures of 900–1200 °C, but there was significant degradation in the tensile strength of 9Cr-ODS steel claddings above 1200 °C. This degradation was attributed to grain boundary sliding deformation with γ/δ transformation, which is associated with reduced ductility. By contrast, the tensile strength of recrystallized 12Cr-ODS and FeCrAl-ODS steel claddings retained its high value above 1200 °C, unlike the other tested materials.

  10. Ultra-high temperature tensile properties of ODS steel claddings under severe accident conditions

    Science.gov (United States)

    Yano, Y.; Tanno, T.; Oka, H.; Ohtsuka, S.; Inoue, T.; Kato, S.; Furukawa, T.; Uwaba, T.; Kaito, T.; Ukai, S.; Oono, N.; Kimura, A.; Hayashi, S.; Torimaru, T.

    2017-04-01

    Ultra-high temperature ring tensile tests were performed to investigate the tensile behavior of oxide dispersion strengthened (ODS) steel claddings and wrapper materials under severe accident conditions with temperatures ranging from room temperature to 1400 °C which is close to the melting point of core materials. The experimental results showed that the tensile strength of 9Cr-ODS steel claddings was highest in the core materials at ultra-high temperatures of 900-1200 °C, but there was significant degradation in the tensile strength of 9Cr-ODS steel claddings above 1200 °C. This degradation was attributed to grain boundary sliding deformation with γ/δ transformation, which is associated with reduced ductility. By contrast, the tensile strength of recrystallized 12Cr-ODS and FeCrAl-ODS steel claddings retained its high value above 1200 °C, unlike the other tested materials.

  11. Diamond dispersed cemented carbide produced without using ultra high pressure equipment

    International Nuclear Information System (INIS)

    Moriguchi, H.; Tsuzuki, K.; Ikegaya, A.

    2001-01-01

    We have developed a composite material of dispersed diamond particles in cemented carbide without using ultra high pressure equipment. The developed diamond dispersed cemented carbide combines the excellent properties of cemented carbide with diamond and also provides 1.5 times improved fracture toughness over that of cemented carbide. They also show 10 times higher wear resistance over that of cemented carbide in a wear resistance test against bearing steel, and 5 times greater grindability than diamond compacts. Because ultra high pressure equipment is not used to produce the developed material, large compacts over 100 mm in diameter can be manufactured. The developed material showed 10-25 times higher wear resistance in real use as wear-resistant tools such as centerless blades and work-rests. (author)

  12. Ultra-High Field Magnets for X-Ray and Neutron Scattering using High Temperature Superconductors

    Energy Technology Data Exchange (ETDEWEB)

    Winn, Barry L. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Broholm, C. [Johns Hopkins Univ., Baltimore, MD (United States); Bird, M. [Florida State Univ., Tallahassee, FL (United States). National High Magnetic Field Lab. (MagLab); Breneman, Bruce C. [General Atomics, San Diego, CA (United States); Coffey, Michael [Cryomagnetics, Oak Ridge, TN (United States); Cutler, Roy I. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Duckworth, Robert C. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Erwin, R. [National Inst. of Standards and Technology (NIST), Gaithersburg, MD (United States); Hahn, Seungyong [Florida State Univ., Tallahassee, FL (United States). National High Magnetic Field Lab. (MagLab); Hernandez, Yamali [National Inst. of Standards and Technology (NIST), Gaithersburg, MD (United States); Herwig, Kenneth W. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Holland, Leo D. [General Atomics, San Diego, CA (United States); Lonergan, Kevin M. [Oxford Instruments, Abingdon (United Kingdom); Melhem, Ziad [Oxford Instruments, Abingdon (United Kingdom); Minter, Stephen J. [Cryomagnetics, Oak Ridge, TN (United States); Nelson, C. [Brookhaven National Lab. (BNL), Upton, NY (United States); Paranthaman, M. Parans [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Pierce, Josh [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Ruff, Jacob [Cornell Univ., Ithaca, NY (United States); Shen, Tengming [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Sherline, Todd E. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Smeibidl, Peter G. [Helmholtz-Zentrum Berlin (HZB), (Germany); Tennant, David [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); van der Laan, Danko [Advanced Conductor Technologies, LLC, Boulder, CO (United States); Wahle, Robert J. [Helmholtz-Zentrum Berlin (HZB), (Germany); Zhang, Yifei [SuperPower, Inc., Schenectady, NY (United States)

    2017-01-01

    X-ray and neutron scattering techniques are capable of acquiring information about the structure and dynamics of quantum matter. However, the high-field magnet systems currently available at x-ray and neutron scattering facilities in the United States are limited to fields of 16 tesla (T) at maximum, which precludes applications that require and/or study ultra-high field states of matter. This gap in capability—and the need to address it—is a central conclusion of the 2005 National Academy of Sciences report by the Committee on Opportunities in High Magnetic Field Science. To address this gap, we propose a magnet development program that would more than double the field range accessible to scattering experiments. With the development and use of new ultra-high field–magnets, the program would bring into view new worlds of quantum matter with profound impacts on our understanding of advanced electronic materials.

  13. High resolution separations of charge variants and disulfide isomers of monoclonal antibodies and antibody drug conjugates using ultra-high voltage capillary electrophoresis with high electric field strength.

    Science.gov (United States)

    Henley, W Hampton; He, Yan; Mellors, J Scott; Batz, Nicholas G; Ramsey, J Michael; Jorgenson, James W

    2017-11-10

    Ultra-high voltage capillary electrophoresis with high electric field strength has been applied to the separation of the charge variants, drug conjugates, and disulfide isomers of monoclonal antibodies. Samples composed of many closely related species are difficult to resolve and quantify using traditional analytical instrumentation. High performance instrumentation can often save considerable time and effort otherwise spent on extensive method development. Ideally, the resolution obtained for a given CE buffer system scales with the square root of the applied voltage. Currently available commercial CE instrumentation is limited to an applied voltage of approximately 30kV and a maximum electric field strength of 1kV/cm due to design limitations. The instrumentation described here is capable of safely applying potentials of at least 120kV with electric field strengths over 2000V/cm, potentially doubling the resolution of the best conventional CE buffer/capillary systems while decreasing analysis time in some applications. Separations of these complex mixtures using this new instrumentation demonstrate the potential of ultra-high voltage CE to identify the presence of previously unresolved components and to reduce analysis time for complex mixtures of antibody variants and drug conjugates. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Specific features of high-cycle and ultra-high-cycle fatigue

    Czech Academy of Sciences Publication Activity Database

    Lukáš, Petr; Kunz, Ludvík

    2002-01-01

    Roč. 25, - (2002), s. 747-753 ISSN 8756-758X R&D Projects: GA AV ČR KSK1010104; GA AV ČR IAA2041002 Institutional research plan: CEZ:AV0Z2041904 Keywords : ultra high cycle fatigue * fatigue mechanisms * cyclic plastic deformation Subject RIV: JL - Materials Fatigue, Friction Mechanics Impact factor: 0.701, year: 2002

  15. A novel ultra-high vacuum manipulator with six degrees of freedom

    International Nuclear Information System (INIS)

    Auciello, O.; Lulich, C.; Alonso, E.V.; Baragiola, R.A.

    1977-01-01

    An ultra-high vacuum goniometer of novel design for use in experiments with ion beams is described. The goniometer uses a wire system to transmit movements, is bakeable to 200 0 C and is reproducible in its angular positions to within 1.3 X 10 -4 rad (0.008 0 ). It allows a sample to be rotated around two axes over 360 0 , around a third over 180 0 , and to be translated along three perpendicular axes. (Auth.)

  16. Evaluation of environmental degradation effects in morphology of ultra-high molecular weight polyethylene (UHMWPE) fibers

    International Nuclear Information System (INIS)

    Vivas, Viviane; Zylberberg, Marcel P.; Cardoso, Andre Luis V.; Pereira, Iaci M.; Weber, Ricardo P.; Suarez, Joao C. Miguez

    2015-01-01

    This study aims to evaluate changes in the morphology of ultra-high molecular weight polyethylene fiber (UHMWPE), before and after exposure to environmental agents. Fibers produced by two different manufacturers were analyzed. To characterize the morphology, we used the technique of small angle x-ray scattering (SAXS). The results demonstrate that the original morphology of the fibers was UHMWPE affected by the defects caused by exposure to environmental agents. (author)

  17. Measurement of ultra-high energy cosmic rays: An experimental summary and prospects

    Directory of Open Access Journals (Sweden)

    Fukushima M.

    2013-06-01

    Full Text Available Measurements of Ultra-High Energy Cosmic Rays achieved remarkable progress in the last 10 years. Physicists, gathered from around the world in the symposium UHECR-2012 held at CERN on February 13-16 2012, reported their most up-to-date observations, discussed the meaning of their findings, and identified remaining problems and future challenges in this field. This paper is a part of the symposium proceedings on the experimental summary and future prospects of the UHECR study.

  18. Research and Application of WCF Technology in Data Acquisition of Ultra-high Speed Packaging Machine

    Directory of Open Access Journals (Sweden)

    Qian Jie

    2016-01-01

    Full Text Available By introducing WCF technology on data acquisition of ultra-high speed packaging machine, data acquisition system reads dates of machine in polling mode through the WCF client, which can achieve accurate data collection, and effectively isolate the data acquisition system and the machine control system. It enhances the security of data interaction between systems, but also reduces the coupling degree between systems.

  19. Inactivation of Bacillus spores inoculated in milk by Ultra High Pressure Homogenization.

    Science.gov (United States)

    Amador Espejo, Genaro Gustavo; Hernández-Herrero, M M; Juan, B; Trujillo, A J

    2014-12-01

    Ultra High-Pressure Homogenization treatments at 300 MPa with inlet temperatures (Ti) of 55, 65, 75 and 85 °C were applied to commercial Ultra High Temperature treated whole milk inoculated with Bacillus cereus, Bacillus licheniformis, Bacillus sporothermodurans, Bacillus coagulans, Geobacillus stearothermophilus and Bacillus subtilis spores in order to evaluate the inactivation level achieved. Ultra High-Pressure Homogenization conditions at 300 MPa with Ti = 75 and 85 °C were capable of a spore inactivation of ∼5 log CFU/mL. Furthermore, under these processing conditions, commercial sterility (evaluated as the complete inactivation of the inoculated spores) was obtained in milk, with the exception of G. stearothermophilus and B. subtilis treated at 300 MPa with Ti = 75 °C. The results showed that G. stearothermophilus and B. subtilis have higher resistance to the Ultra High-Pressure Homogenization treatments applied than the other microorganisms inoculated and that a treatment performed at 300 MPa with Ti = 85 °C was necessary to completely inactivate these microorganisms at the spore level inoculated (∼1 × 10(6) CFU/mL). Besides, a change in the resistance of B. licheniformis, B. sporothermodurans, G. stearothermophilus and B. subtilis spores was observed as the inactivation obtained increased remarkably in treatments performed with Ti between 65 and 75 °C. This study provides important evidence of the suitability of UHPH technology for the inactivation of spores in high numbers, leading to the possibility of obtaining commercially sterile milk. Copyright © 2014 Elsevier Ltd. All rights reserved.

  20. Patterns of white matter microstructure in individuals at ultra-high-risk for psychosis

    DEFF Research Database (Denmark)

    Krakauer, K; Ebdrup, B H; Glenthøj, B Y

    2017-01-01

    BACKGROUND: Individuals at ultra-high-risk (UHR) for psychosis present with emerging symptoms and decline in functioning. Previous univariate analyses have indicated widespread white matter (WM) aberrations in multiple brain regions in UHR individuals and patients with schizophrenia. Using multiv......, MO, and higher RD. CONCLUSIONS: UHR individuals demonstrate complex brain patterns of WM abnormalities. Despite the subtle psychopathology of UHR individuals, aberrations in WM appear associated with positive and negative symptoms as well as level of functioning....

  1. Silver Nanoparticles Modification of Ultra High Molecular Weight Polyethylene in Non-Aqueous Medium

    OpenAIRE

    V. N. Glushko; L. I. Blokhina; E. E. Anisimova; M. V. Bogdanovskaya; V. I. Kozhukhov; T. A. Cherdyntseva

    2016-01-01

    A series of experiments for obtaining modified with silver nanoparticles ultra-high molecular weight polyethylene (UHMWPE) is done. Optimal precursors are silver trifluoroacetate, silver nitrate and silver methanesulfonate. Three variants of UHMWPE modification is studied: 1) the polyol synthesis, 2) polymer processing silver nanoparticle colloid and 3) reduction of silver salt solution in the UHMWPE polymer matrix. It is found that the last method is optimal. The specific surface of obtained...

  2. Ground Glass Pozzolan in Conventional, High, and Ultra-High Performance Concrete

    OpenAIRE

    Tagnit-Hamou Arezki; Zidol Ablam; Soliman Nancy; Deschamps Joris; Omran Ahmed

    2018-01-01

    Ground-glass pozzolan (G) obtained by grinding the mixed-waste glass to same fineness of cement can act as a supplementary-cementitious material (SCM), given that it is an amorphous and a pozzolanic material. The G showed promising performances in different concrete types such as conventional concrete (CC), high-performance concrete (HPC), and ultra-high performance concrete (UHPC). The current paper reports on the characteristics and performance of G in these concrete types. The use of G pro...

  3. RECENT ADVANCES IN ULTRA-HIGH PERFORMANCE LIQUID CHROMATOGRAPHY FOR THE ANALYSIS OF TRADITIONAL CHINESE MEDICINE

    Science.gov (United States)

    Huang, Huilian; Liu, Min; Chen, Pei

    2014-01-01

    Traditional Chinese medicine has been widely used for the prevention and treatment of various diseases for thousands of years in China. Ultra-high performance liquid chromatography (UHPLC) is a relatively new technique offering new possibilities. This paper reviews recent developments in UHPLC in the separation and identification, fingerprinting, quantification, and metabolism of traditional Chinese medicine. Recently, the combination of UHPLC with MS has improved the efficiency of the analysis of these materials. PMID:25045170

  4. Physics of Eclipsing Binaries: Modelling in the new era of ultra-high precision photometry

    OpenAIRE

    Pavlovski, K.; Bloemen, S.; Degroote, P.; Conroy, K.; Hambleton, Kelly; Giammarco, J.M.; Pablo, H.; Prša, A.; Tkachenko, A.; Torres, G.

    2013-01-01

    Recent ultra-high precision observations of eclipsing binaries, especially data acquired by the Kepler satellite, have made accurate light curve modelling increasingly challenging but also more rewarding. In this contribution, we discuss low-amplitude signals in light curves that can now be used to derive physical information about eclipsing binaries but that were unaccessible before the Kepler era. A notable example is the detection of Doppler beaming, which leads to an increase in flux when...

  5. Evaluating strength at ultra-high temperatures-Methods and results

    International Nuclear Information System (INIS)

    Voelkl, Rainer; Fischer, Bernd; Beschliesser, Manuel; Glatzel, Uwe

    2008-01-01

    Proprietary equipment for mechanical testing at ultra-high temperatures by ohmic heating is outlined. Strain is measured with a video extensometer with an accuracy of up to Δε-bar∼±0.00025%. Stability and accuracy of the test system are evaluated on Pt- and refractory alloys. These specially designed and built test facilities are compared to commercially available high-vacuum test chambers with tungsten heater

  6. The lateral characteristics of several ultra-high energy photon and hadron families

    International Nuclear Information System (INIS)

    Buja, Z.; Gladysz, E.; Mazurkiewicz, J.; Mikocki, S.; Szarska, M.; Zawiejski, L.

    1980-01-01

    In a thick lead X-ray film emulsion chamber of the Experiment Pamir, 8 ultra-high energy photon and hadron families were detected. They are considered to be almost ''pure'' families. The compound lateral characteristics for photon families indicate an existence of two groups of particles which have different average transverse momenta. A quite well visible azimuthal asymmetry in the number and transverse momenta values of produced particles is observed. (author)

  7. Point source search techniques in ultra high energy gamma ray astronomy

    International Nuclear Information System (INIS)

    Alexandreas, D.E.; Biller, S.; Dion, G.M.; Lu, X.Q.; Yodh, G.B.; Berley, D.; Goodman, J.A.; Haines, T.J.; Hoffman, C.M.; Horch, E.; Sinnis, C.; Zhang, W.

    1993-01-01

    Searches for point astrophysical sources of ultra high energy (UHE) gamma rays are plagued by large numbers of background events from isotropic cosmic rays. Some of the methods that have been used to estimate the expected number of background events coming from the direction of a possible source are found to contain biases. Search techniques that avoid this problem are described. There is also a discussion of how to optimize the sensitivity of a search to emission from a point source. (orig.)

  8. Modelling of radiation losses for ion acceleration at ultra-high laser intensities

    Directory of Open Access Journals (Sweden)

    Capdessus Remi

    2013-11-01

    Full Text Available Radiation losses of charged particles can become important in ultra high intensity laser plasma interaction. This process is described by the radiation back reaction term in the electron equation of motion. This term is implemented in the relativistic particle-in-cell code by using a renormalized Lorentz-Abraham-Dirac model. In the hole boring regime case of laser ion acceleration it is shown that radiation losses results in a decrease of the piston velocity.

  9. Arc Shape Characteristics with Ultra-High-Frequency Pulsed Arc Welding

    Directory of Open Access Journals (Sweden)

    Mingxuan Yang

    2017-01-01

    Full Text Available Arc plasma possesses a constriction phenomenon with a pulsed current. The constriction is created by the Lorentz force, the radial electromagnetic force during arc welding, which determines the energy distribution of the arc plasma. Welding experiments were carried out with ultra-high-frequency pulsed arc welding (UHFP-AW. Ultra-high-speed camera observations were produced for arc surveillance. Hue-saturation-intensity (HSI image analysis was used to distinguish the regions of the arc plasma that represented the heat energy distribution. The measurement of arc regions indicated that, with an ultra-high-frequency pulsed arc, the constriction was not only within the decreased arc geometry, but also within the constricted arc core region. This can be checked by the ratio of the core region to the total area. The arc core region expanded significantly at 40 kHz at 60 A. A current level of 80 A caused a decrease in the total region of the arc. Meanwhile, the ratio of the core region to the total increased. It can be concluded that arc constriction depends on the increased area of the core region with the pulsed current (>20 kHz.

  10. A Manganin Thin Film Ultra-High Pressure Sensor for Microscale Detonation Pressure Measurement

    Directory of Open Access Journals (Sweden)

    Guodong Zhang

    2018-03-01

    Full Text Available With the development of energetic materials (EMs and microelectromechanical systems (MEMS initiating explosive devices, the measurement of detonation pressure generated by EMs in the microscale has become a pressing need. This paper develops a manganin thin film ultra-high pressure sensor based on MEMS technology for measuring the output pressure from micro-detonator. A reliable coefficient is proposed for designing the sensor’s sensitive element better. The sensor employs sandwich structure: the substrate uses a 0.5 mm thick alumina ceramic, the manganin sensitive element with a size of 0.2 mm × 0.1 mm × 2 μm and copper electrodes of 2 μm thick are sputtered sequentially on the substrate, and a 25 μm thick insulating layer of polyimide is wrapped on the sensitive element. The static test shows that the piezoresistive coefficient of manganin thin film is 0.0125 GPa−1. The dynamic experiment indicates that the detonation pressure of micro-detonator is 12.66 GPa, and the response time of the sensor is 37 ns. In a word, the sensor developed in this study is suitable for measuring ultra-high pressure in microscale and has a shorter response time than that of foil-like manganin gauges. Simultaneously, this study could be beneficial to research on ultra-high-pressure sensors with smaller size.

  11. Simulation of press-forming for automobile part using ultra high tension steel

    Directory of Open Access Journals (Sweden)

    Tanabe I.

    2012-08-01

    Full Text Available In recent years, ultra high tension steel has gradually been used in the automobile industry. The development of press-forming technology is now essential by reason of its high productivity and high product quality. In this study, tensile tests were performed with a view to understanding the material properties. Press-forming tests were then carried out with regard to the behaviors of spring back and deep-drawability, and manufacturing a real product. The ultra high tension steel used in the experiments had a thickness of 1 mm and a tensile strength of 1000 MPa. Finally, simulations of spring back, deep-drawability and manufacturing a real product in ultra high tension steel were conducted and evaluated in order to calculate the optimum-press-forming conditions and the optimum shape of the die. FEM with non-linear and dynamic analysis using Euler-Lagrange’s element was used for the simulations. It is concluded from the results that (1 the simulations conformed to the results of the experiments (2 the simulations proved very effective for calculating the optimum press conditions and die shape.

  12. Ultra-high throughput real-time instruments for capturing fast signals and rare events

    Science.gov (United States)

    Buckley, Brandon Walter

    Wide-band signals play important roles in the most exciting areas of science, engineering, and medicine. To keep up with the demands of exploding internet traffic, modern data centers and communication networks are employing increasingly faster data rates. Wide-band techniques such as pulsed radar jamming and spread spectrum frequency hopping are used on the battlefield to wrestle control of the electromagnetic spectrum. Neurons communicate with each other using transient action potentials that last for only milliseconds at a time. And in the search for rare cells, biologists flow large populations of cells single file down microfluidic channels, interrogating them one-by-one, tens of thousands of times per second. Studying and enabling such high-speed phenomena pose enormous technical challenges. For one, parasitic capacitance inherent in analog electrical components limits their response time. Additionally, converting these fast analog signals to the digital domain requires enormous sampling speeds, which can lead to significant jitter and distortion. State-of-the-art imaging technologies, essential for studying biological dynamics and cells in flow, are limited in speed and sensitivity by finite charge transfer and read rates, and by the small numbers of photo-electrons accumulated in short integration times. And finally, ultra-high throughput real-time digital processing is required at the backend to analyze the streaming data. In this thesis, I discuss my work in developing real-time instruments, employing ultrafast optical techniques, which overcome some of these obstacles. In particular, I use broadband dispersive optics to slow down fast signals to speeds accessible to high-bit depth digitizers and signal processors. I also apply telecommunication multiplexing techniques to boost the speeds of confocal fluorescence microscopy. The photonic time stretcher (TiSER) uses dispersive Fourier transformation to slow down analog signals before digitization and

  13. Ultra-high performance fiber-reinforced concrete (UHPFRC) for infrastructure rehabilitation Volume II : behavior of ultra-high strength concrete bridge deck panels compared to conventional stay-in-place deck panels

    Science.gov (United States)

    2017-08-01

    The remarkable features of ultra-high performance concrete (UHPC) have been reported. Its application in bridge construction has been an active research area in recent years, attributed to its higher compressive strength, higher ductility and reduced...

  14. Set-up of a high-resolution 300 mK atomic force microscope in an ultra-high vacuum compatible "3He/10 T cryostat

    International Nuclear Information System (INIS)

    Allwörden, H. von; Ruschmeier, K.; Köhler, A.; Eelbo, T.; Schwarz, A.; Wiesendanger, R.

    2016-01-01

    The design of an atomic force microscope with an all-fiber interferometric detection scheme capable of atomic resolution at about 500 mK is presented. The microscope body is connected to a small pumped "3He reservoir with a base temperature of about 300 mK. The bakeable insert with the cooling stage can be moved from its measurement position inside the bore of a superconducting 10 T magnet into an ultra-high vacuum chamber, where the tip and sample can be exchanged in situ. Moreover, single atoms or molecules can be evaporated onto a cold substrate located inside the microscope. Two side chambers are equipped with standard surface preparation and surface analysis tools. The performance of the microscope at low temperatures is demonstrated by resolving single Co atoms on Mn/W(110) and by showing atomic resolution on NaCl(001).

  15. Set-up of a high-resolution 300 mK atomic force microscope in an ultra-high vacuum compatible {sup 3}He/10 T cryostat

    Energy Technology Data Exchange (ETDEWEB)

    Allwörden, H. von; Ruschmeier, K.; Köhler, A.; Eelbo, T.; Schwarz, A., E-mail: aschwarz@physnet.uni-hamburg.de; Wiesendanger, R. [Department of Physics, University of Hamburg, Jungiusstrasse 11, 20355 Hamburg (Germany)

    2016-07-15

    The design of an atomic force microscope with an all-fiber interferometric detection scheme capable of atomic resolution at about 500 mK is presented. The microscope body is connected to a small pumped {sup 3}He reservoir with a base temperature of about 300 mK. The bakeable insert with the cooling stage can be moved from its measurement position inside the bore of a superconducting 10 T magnet into an ultra-high vacuum chamber, where the tip and sample can be exchanged in situ. Moreover, single atoms or molecules can be evaporated onto a cold substrate located inside the microscope. Two side chambers are equipped with standard surface preparation and surface analysis tools. The performance of the microscope at low temperatures is demonstrated by resolving single Co atoms on Mn/W(110) and by showing atomic resolution on NaCl(001).

  16. High-energy green supercapacitor driven by ionic liquid electrolytes as an ultra-high stable next-generation energy storage device

    Science.gov (United States)

    Thangavel, Ranjith; Kannan, Aravindaraj G.; Ponraj, Rubha; Thangavel, Vigneysh; Kim, Dong-Won; Lee, Yun-Sung

    2018-04-01

    Development of supercapacitors with high energy density and long cycle life using sustainable materials for next-generation applications is of paramount importance. The ongoing challenge is to elevate the energy density of supercapacitors on par with batteries, while upholding the power and cyclability. In addition, attaining such superior performance with green and sustainable bio-mass derived compounds is very crucial to address the rising environmental concerns. Herein, we demonstrate the use of watermelon rind, a bio-waste from watermelons, towards high energy, and ultra-stable high temperature green supercapacitors with a high-voltage ionic liquid electrolyte. Supercapacitors assembled with ultra-high surface area, hierarchically porous carbon exhibits a remarkable performance both at room temperature and at high temperature (60 °C) with maximum energy densities of ∼174 Wh kg-1 (25 °C), and 177 Wh kg-1 (60 °C) - based on active mass of both electrodes. Furthermore, an ultra-high specific power of ∼20 kW kg-1 along with an ultra-stable cycling performance with 90% retention over 150,000 cycles has been achieved even at 60 °C, outperforming supercapacitors assembled with other carbon based materials. These results demonstrate the potential to develop high-performing, green energy storage devices using eco-friendly materials for next generation electric vehicles and other advanced energy storage systems.

  17. Ultra High Temperature and Multifunctional Ceramic Matrix Composite – Coating Systems for Light-Weight Space and Aero Systems

    Data.gov (United States)

    National Aeronautics and Space Administration — Revolutionary ultra-high temperature, high mechanical loading capable, oxidation resistant, durable ceramic coatings and light-weight fiber-reinforced Ceramic Matrix...

  18. Pre-pulse inhibition and striatal dopamine in subjects at an ultra-high risk for psychosis

    NARCIS (Netherlands)

    de Koning, Mariken B.; Bloemen, Oswald J. N.; van Duin, Esther D. A.; Booij, Jan; Abel, Kathryn M.; de Haan, Lieuwe; Linszen, Don H.; van Amelsvoort, Thérèse A. M. J.

    2014-01-01

    Reduced prepulse inhibition (PPI) of the acoustic startle response is thought to represent a robust biomarker in schizophrenia. Reduced PPI has been demonstrated in subjects at ultra high risk (UHR) for developing psychosis. Imaging studies report disruption of striatal dopaminergic

  19. Flexible mechanoprosthesis made from woven ultra-high-molecular-weight polyethylene fibres : proof of concept in a chronic sheep model

    NARCIS (Netherlands)

    Basir, Amir; Grobben, Remco B.; Cramer, Maarten Jan; van Herwaarden, Joost A.; Vink, Aryan; Pasterkamp, Gerard; Kluin, Jolanda; Gründeman, Paul F.

    2017-01-01

    OBJECTIVES: Ultra-high-molecular-weight polyethylene (UHMWPE) fibres are flexible, have high tensile strength, and platelet and bacterial adhesion is low. Therefore, UHMWPE may overcome limitations of current mechanical valves and bioprostheses. In this study, the biocompatibility and functionality

  20. Advanced processing of gallium nitride and gallium nitride-based devices: Ultra-high temperature annealing and implantation incorporation

    Science.gov (United States)

    Yu, Haijiang

    This dissertation is focused on three fields: ultra-high temperature annealing of GaN, activation of implanted GaN and the implantation incorporation into AlGaN/GaN HEMT processing, with an aim to increase the performance, manufacturability and reliability of AlGaN/GaN HEMTs. First, the ultra high temperature (around 1500°C) annealing of MOCVD grown GaN on sapphire has been studied, and a thermally induced threading dislocation (TD) motion and reaction are reported. Using a rapid thermal annealing (RTA) approach capable of heating 2 inch wafers to around 1500°C with 100 bar N2 over-pressure, evidence of dislocation motion was first observed in transmission electron microscopy (TEM) micrographs of both planar and patterned GaN films protected by an AIN capping layer. An associated decrease in x-ray rocking curve (XRC) full-width-half-maximum (FWHM) was also observed for both the symmetric and asymmetric scans. After annealing, the AIN capping layer remained intact, and optical measurements showed no degradation of the opto-electronic properties of the films. Then activation annealing of Si implants in MOCVD grown GaN has been studied for use in ohmic contacts. Si was implanted in semi-insulating GaN at 100 keV with doses from 5 x 1014 cm-2 to 1.5 x 1016 cm-2. Rapid thermal annealing at 1500°C with 100 bar N2 over-pressure was used for dopant activation, resulting in a minimum sheet resistance of 13.9 O/square for a dose of 7 x 1015 cm-2. Secondary ion mass spectroscopy measurements showed a post-activation broadening of the dopant concentration peak by 20 nm (at half the maximum), while X-Ray triple axis o-2theta scans indicated nearly complete implant damage recovery. Transfer length method measurements of the resistance of Ti/Al/Ni/Au contacts to activated GaN:Si (5 x 1015 cm-2 at 100 keV) indicated lowest contact resistances of 0.07 Omm and 0.02 Omm for as-deposited and subsequently annealed contacts, respectively. Finally, the incorporation of Si implantation

  1. Investigation and basic evaluation for ultra-high burnup fuel cladding material

    International Nuclear Information System (INIS)

    Ioka, Ikuo; Nagase, Fumihisa; Futakawa, Masatoshi; Kiuchi, Kiyoshi

    2001-03-01

    In ultra-high burnup of the power reactor, it is an essential problem to develop the cladding with excellent durability. First, development history and approach of the safety assessment of Zircaloy for the high burnup fuel were summarized in the report. Second, the basic evaluation and investigation were carried out on the material with high practicability in order to select the candidate materials for the ultra-high burnup fuel. In addition, the basic research on modification technology of the cladding surface was carried out from the viewpoint of the addition of safety margin as a cladding. From the development history of the zirconium alloy including the Zircaloy, it is hard to estimate the results of in-pile test from those of the conventional corrosion test (out-pile test). Therefore, the development of the new testing technology that can simulate the actual environment and the elucidation of the corrosion-controlling factor of the cladding are desired. In cases of RIA (Reactivity Initiated Accident) and LOCA (Loss of Coolant Accident), it seems that the loss of ductility in zirconium alloys under heavy irradiation and boiling of high temperature water restricts the extension of fuel burnup. From preliminary evaluation on the high corrosion-resistance materials (austenitic stainless steel, iron or nickel base superalloys, titanium alloy, niobium alloy, vanadium alloy and ferritic stainless steel), stabilized austenitic stainless steels with a capability of future improvement and high-purity niobium alloys with a expectation of the good corrosion resistance were selected as candidate materials of ultra-high burnup cladding. (author)

  2. Kernel based methods for accelerated failure time model with ultra-high dimensional data

    Directory of Open Access Journals (Sweden)

    Jiang Feng

    2010-12-01

    Full Text Available Abstract Background Most genomic data have ultra-high dimensions with more than 10,000 genes (probes. Regularization methods with L1 and Lp penalty have been extensively studied in survival analysis with high-dimensional genomic data. However, when the sample size n ≪ m (the number of genes, directly identifying a small subset of genes from ultra-high (m > 10, 000 dimensional data is time-consuming and not computationally efficient. In current microarray analysis, what people really do is select a couple of thousands (or hundreds of genes using univariate analysis or statistical tests, and then apply the LASSO-type penalty to further reduce the number of disease associated genes. This two-step procedure may introduce bias and inaccuracy and lead us to miss biologically important genes. Results The accelerated failure time (AFT model is a linear regression model and a useful alternative to the Cox model for survival analysis. In this paper, we propose a nonlinear kernel based AFT model and an efficient variable selection method with adaptive kernel ridge regression. Our proposed variable selection method is based on the kernel matrix and dual problem with a much smaller n × n matrix. It is very efficient when the number of unknown variables (genes is much larger than the number of samples. Moreover, the primal variables are explicitly updated and the sparsity in the solution is exploited. Conclusions Our proposed methods can simultaneously identify survival associated prognostic factors and predict survival outcomes with ultra-high dimensional genomic data. We have demonstrated the performance of our methods with both simulation and real data. The proposed method performs superbly with limited computational studies.

  3. Ultra high spatial and temporal resolution breast imaging at 7T.

    Science.gov (United States)

    van de Bank, B L; Voogt, I J; Italiaander, M; Stehouwer, B L; Boer, V O; Luijten, P R; Klomp, D W J

    2013-04-01

    There is a need to obtain higher specificity in the detection of breast lesions using MRI. To address this need, Dynamic Contrast-Enhanced (DCE) MRI has been combined with other structural and functional MRI techniques. Unfortunately, owing to time constraints structural images at ultra-high spatial resolution can generally not be obtained during contrast uptake, whereas the relatively low spatial resolution of functional imaging (e.g. diffusion and perfusion) limits the detection of small lesions. To be able to increase spatial as well as temporal resolution simultaneously, the sensitivity of MR detection needs to increase as well as the ability to effectively accelerate the acquisition. The required gain in signal-to-noise ratio (SNR) can be obtained at 7T, whereas acceleration can be obtained with high-density receiver coil arrays. In this case, morphological imaging can be merged with DCE-MRI, and other functional techniques can be obtained at higher spatial resolution, and with less distortion [e.g. Diffusion Weighted Imaging (DWI)]. To test the feasibility of this concept, we developed a unilateral breast coil for 7T. It comprises a volume optimized dual-channel transmit coil combined with a 30-channel receive array coil. The high density of small coil elements enabled efficient acceleration in any direction to acquire ultra high spatial resolution MRI of close to 0.6 mm isotropic detail within a temporal resolution of 69 s, high spatial resolution MRI of 1.5 mm isotropic within an ultra high temporal resolution of 6.7 s and low distortion DWI at 7T, all validated in phantoms, healthy volunteers and a patient with a lesion in the right breast classified as Breast Imaging Reporting and Data System (BI-RADS) IV. Copyright © 2012 John Wiley & Sons, Ltd.

  4. Design and Fabrication of a Piezoresistive Pressure Sensor for Ultra High Temperature Environment

    International Nuclear Information System (INIS)

    Zhao, L B; Zhao, Y L; Jiang, Z D

    2006-01-01

    In order to solve the pressure measurement problem in the harsh environment, a piezoresistive pressure sensor has been developed, which can be used under high temperature above 200 deg. C and is able to endure instantaneous ultra high temperature (2000deg. C, duration≤2s) impact. Based on the MEMS (Micro Electro-Mechanical System) and integrated circuit technology, the piezoresistive pressure sensor's sensitive element was fabricated and constituted by silicon substrate, a thin buried silicon dioxide layer, four p-type resistors in the measuring circuit layer by boron ion implantation and photolithography, the top SiO2 layer by oxidation, stress matching Si3N4 layer, and a Ti-Pt-Au beam lead layer for connecting p-type resistors by sputtering. In order to decrease the leak-current influence to sensor in high temperature above 200deg. C, the buried SiO2 layer with the thickness 367 nm was fabricated by the SIMOX (Separation by Implantation of Oxygen) technology, which was instead of p-n junction to isolate the upper measuring circuit layer from Si substrate. In order to endure instantaneous ultra high temperature impact, the mechanical structure with cantilever and diaphragm and transmitting beam was designed. By laser welding and high temperature packaging technology, the high temperature piezoresistive pressure sensor was fabricated with range of 120MPa. After the thermal compensation, the sensor's thermal zero drift k 0 and thermal sensitivity drift k s were easy to be less than 3x10 -4 FS/deg. C. The experimental results show that the developed piezoresistive pressure sensor has good performances under high temperature and is able to endure instantaneous ultra high temperature impact, which meets the requirements of modern industry, such as aviation, oil, engine, etc

  5. Multifunctional ultra-high vacuum apparatus for studies of the interactions of chemical warfare agents on complex surfaces

    International Nuclear Information System (INIS)

    Wilmsmeyer, Amanda R.; Morris, John R.; Gordon, Wesley O.; Mantooth, Brent A.; Lalain, Teri A.; Davis, Erin Durke

    2014-01-01

    A fundamental understanding of the surface chemistry of chemical warfare agents is needed to fully predict the interaction of these toxic molecules with militarily relevant materials, catalysts, and environmental surfaces. For example, rules for predicting the surface chemistry of agents can be applied to the creation of next generation decontaminants, reactive coatings, and protective materials for the warfighter. Here, we describe a multifunctional ultra-high vacuum instrument for conducting comprehensive studies of the adsorption, desorption, and surface chemistry of chemical warfare agents on model and militarily relevant surfaces. The system applies reflection-absorption infrared spectroscopy, x-ray photoelectron spectroscopy, and mass spectrometry to study adsorption and surface reactions of chemical warfare agents. Several novel components have been developed to address the unique safety and sample exposure challenges that accompany the research of these toxic, often very low vapor pressure, compounds. While results of vacuum-based surface science techniques may not necessarily translate directly to environmental processes, learning about the fundamental chemistry will begin to inform scientists about the critical aspects that impact real-world applications

  6. Multifunctional ultra-high vacuum apparatus for studies of the interactions of chemical warfare agents on complex surfaces.

    Science.gov (United States)

    Wilmsmeyer, Amanda R; Gordon, Wesley O; Davis, Erin Durke; Mantooth, Brent A; Lalain, Teri A; Morris, John R

    2014-01-01

    A fundamental understanding of the surface chemistry of chemical warfare agents is needed to fully predict the interaction of these toxic molecules with militarily relevant materials, catalysts, and environmental surfaces. For example, rules for predicting the surface chemistry of agents can be applied to the creation of next generation decontaminants, reactive coatings, and protective materials for the warfighter. Here, we describe a multifunctional ultra-high vacuum instrument for conducting comprehensive studies of the adsorption, desorption, and surface chemistry of chemical warfare agents on model and militarily relevant surfaces. The system applies reflection-absorption infrared spectroscopy, x-ray photoelectron spectroscopy, and mass spectrometry to study adsorption and surface reactions of chemical warfare agents. Several novel components have been developed to address the unique safety and sample exposure challenges that accompany the research of these toxic, often very low vapor pressure, compounds. While results of vacuum-based surface science techniques may not necessarily translate directly to environmental processes, learning about the fundamental chemistry will begin to inform scientists about the critical aspects that impact real-world applications.

  7. Multifunctional ultra-high vacuum apparatus for studies of the interactions of chemical warfare agents on complex surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Wilmsmeyer, Amanda R.; Morris, John R. [Department of Chemistry, Virginia Tech, Blacksburg, Virginia 24061 (United States); Gordon, Wesley O.; Mantooth, Brent A.; Lalain, Teri A. [Research and Technology Directorate, U.S. Army Edgewood Chemical Biological Center, Aberdeen Proving Ground, Maryland 21010 (United States); Davis, Erin Durke [OptiMetrics, Inc., Abingdon, Maryland 21009 (United States)

    2014-01-15

    A fundamental understanding of the surface chemistry of chemical warfare agents is needed to fully predict the interaction of these toxic molecules with militarily relevant materials, catalysts, and environmental surfaces. For example, rules for predicting the surface chemistry of agents can be applied to the creation of next generation decontaminants, reactive coatings, and protective materials for the warfighter. Here, we describe a multifunctional ultra-high vacuum instrument for conducting comprehensive studies of the adsorption, desorption, and surface chemistry of chemical warfare agents on model and militarily relevant surfaces. The system applies reflection-absorption infrared spectroscopy, x-ray photoelectron spectroscopy, and mass spectrometry to study adsorption and surface reactions of chemical warfare agents. Several novel components have been developed to address the unique safety and sample exposure challenges that accompany the research of these toxic, often very low vapor pressure, compounds. While results of vacuum-based surface science techniques may not necessarily translate directly to environmental processes, learning about the fundamental chemistry will begin to inform scientists about the critical aspects that impact real-world applications.

  8. CHICSi - a compact ultra-high vacuum compatible detector system for nuclear reaction experiments at storage rings. II. Detectors

    Energy Technology Data Exchange (ETDEWEB)

    Golubev, P.; Avdeichikov, V.; Carlen, L.; Jakobsson, B. E-mail: bo.jakobsson@kosufy.lu.se; Siwek, A.; Veldhuizen, E.J. van; Westerberg, L.; Whitlow, H.J

    2003-03-11

    We describe the detectors for identification of charged particles and fragments in CHICSi, a large solid angle multi-telescope system mounted inside an ultra-high vacuum (UHV), cluster-jet target chamber. CHICSi performs nuclear reaction experiments at storage rings. The telescopes consist of a first very thin, 10-14 {mu}m Si detector, a second 300 {mu}m (or possibly 500 {mu}m) ion implanted Si detector supplemented by a 6 mm GSO(Ce) scintillator read out by a photodiode (PD) or by a third 300 {mu}m Si detector. The telescopes provide full charge separation up to Z=17 and mass resolution up to A=9 in the energy range 0.7-60A MeV. The thin p-i-n diode detector, etched out from a 280 {mu}m Si wafer, and the GSO/PD detector, both exclusively developed for CHICSi, provide an energy resolution {<=}8%, while the standard 300 {mu}m detectors have {<=}2% energy resolution. Radiation stability of the Si detectors is confirmed up to an integrated flux of 10{sup 10} alpha particles. The GSO detector has 70% light collection efficiency with the optical coupling to the PD a simple open, 0.2 mm, gap. A new method, developed to perform absolute energy calibration for the GSO/PD detector is presented.

  9. CHICSi - a compact ultra-high vacuum compatible detector system for nuclear reaction experiments at storage rings. II. Detectors

    International Nuclear Information System (INIS)

    Golubev, P.; Avdeichikov, V.; Carlen, L.; Jakobsson, B.; Siwek, A.; Veldhuizen, E.J. van; Westerberg, L.; Whitlow, H.J.

    2003-01-01

    We describe the detectors for identification of charged particles and fragments in CHICSi, a large solid angle multi-telescope system mounted inside an ultra-high vacuum (UHV), cluster-jet target chamber. CHICSi performs nuclear reaction experiments at storage rings. The telescopes consist of a first very thin, 10-14 μm Si detector, a second 300 μm (or possibly 500 μm) ion implanted Si detector supplemented by a 6 mm GSO(Ce) scintillator read out by a photodiode (PD) or by a third 300 μm Si detector. The telescopes provide full charge separation up to Z=17 and mass resolution up to A=9 in the energy range 0.7-60A MeV. The thin p-i-n diode detector, etched out from a 280 μm Si wafer, and the GSO/PD detector, both exclusively developed for CHICSi, provide an energy resolution ≤8%, while the standard 300 μm detectors have ≤2% energy resolution. Radiation stability of the Si detectors is confirmed up to an integrated flux of