WorldWideScience

Sample records for capture compound mass

  1. Validation of a Liquid Chromatography Tandem Mass Spectrometry Method for Targeted Degradation Compounds of Ethanolamine Used in CO2 Capture: Application to Real Samples

    Directory of Open Access Journals (Sweden)

    Cuzuel Vincent

    2014-09-01

    Full Text Available In the field of greenhouse gas emission, a promising approach consists in CO2 storage and capture. However most of the processes are based on amine solutions which are likely to degrade and produce potentially harmful compounds. So there is a need for analytical methods to identify and quantify these products. Monoethanolamine was used as a model compound for the amines used for CO2 capture. A liquid chromatography tandem mass spectrometry method was developed and validated for the quantification of six products of degradation of monoethanolamine (Glycine, N-(2-hydroxyethylglycine, N-glycylglycine, bicine, N,N′-bis-(2-hydroxyethyl urea (BHE Urea, and diethanolamine that were systematically detected with a LC-MS Scan method in real samples from CO2 capture and storage processes. The main difficulty of this study and its originality ly in the strategy developed to overcome the complexity of the matrix which is a mix of water and amine (70/30: the combined use of deuterated internal standards and a recent chemiometric approach to validate the method, i.e. the accuracy profile. For five compounds it was possible to validate the method with acceptance limits of 20%. This method was then successfully applied to real samples from pilot plant and lab-scale experiments.

  2. Validation of a Liquid Chromatography Tandem Mass Spectrometry Method for Targeted Degradation Compounds of Ethanolamine Used in CO2 Capture: Application to Real Samples

    International Nuclear Information System (INIS)

    In the field of greenhouse gas emission, a promising approach consists in CO2 storage and capture. However most of the processes are based on amine solutions which are likely to degrade and produce potentially harmful compounds. So there is a need for analytical methods to identify and quantify these products. Monoethanolamine was used as a model compound for the amines used for CO2 capture. A liquid chromatography tandem mass spectrometry method was developed and validated for the quantification of six products of degradation of monoethanolamine (Glycine, N-(2-hydroxyethyl)glycine, N-glycylglycine, bicine, N,N'-bis-(2-hydroxyethyl) urea (BHE Urea), and diethanolamine) that were systematically detected with a LC-MS Scan method in real samples from CO2 capture and storage processes. The main difficulty of this study and its originality lie in the strategy developed to overcome the complexity of the matrix which is a mix of water and amine (70/30): the combined use of deuterated internal standards and a recent chemometric approach to validate the method, i.e. the accuracy profile. For five compounds it was possible to validate the method with acceptance limits of 20%. This method was then successfully applied to real samples from pilot plant and lab-scale experiments. (authors)

  3. Improvement of Capture Compound Mass Spectrometry Technology (CCMS) for the Profiling of Human Kinases by Combination with 2D LC-MS/MS

    Science.gov (United States)

    Fischer, Jenny J.; Graebner, Olivia; Dreger, Mathias; Glinski, Mirko; Baumgart, Sabine; Koester, Hubert

    2011-01-01

    An increasingly popular and promising field in functional proteomics is the isolation of proteome subsets based on small molecule-protein interactions. One platform approach in this field are Capture Compounds that contain a small molecule of interest to bind target proteins, a photo-activatable reactivity function to covalently trap bound proteins, and a sorting function to isolate captured protein conjugates from complex biological samples for direct protein identification by liquid chromatography/mass spectrometry (nLC-MS/MS). In this study we used staurosporine as a selectivity group for analysis in HepG2 cells derived from human liver. In the present study, we combined the functional isolation of kinases with different separation workflows of automated split-free nanoflow liquid chromatography prior to mass spectrometric analysis. Two different CCMS setups, CCMS technology combined with 1D LC-MS and 2D LC-MS, were compared regarding the total number of kinase identifications. By extending the chromatographic separation of the tryptic digested captured proteins from 1D LC linear gradients to 2D LC we were able to identify 97 kinases. This result is similar to the 1D LC setup we previously reported but this time 4 times less input material was needed. This makes CCMS of kinases an even more powerful tool for the proteomic profiling of this important protein family. PMID:21941435

  4. Identification of Potential Off-target Toxicity Liabilities of Catechol-O-methyltransferase Inhibitors by Differential Competition Capture Compound Mass Spectrometry.

    Science.gov (United States)

    von Kleist, Lisa; Michaelis, Simon; Bartho, Kathrin; Graebner, Olivia; Schlief, Marén; Dreger, Mathias; Schrey, Anna K; Sefkow, Michael; Kroll, Friedrich; Koester, Hubert; Luo, Yan

    2016-05-26

    Structurally related inhibitors of a shared therapeutic target may differ regarding potential toxicity issues that are caused by different off-target bindings. We devised a differential competition capture compound mass spectrometry (dCCMS) strategy to effectively differentiate off-target profiles. Tolcapone and entacapone are potent inhibitors of catechol-O-methyl transferase (COMT) for the treatment of Parkinson's disease. Tolcapone is also known for its hepatotoxic side effects even though it is therapeutically more potent than entacapone. Here, we identified 3-hydroxyisobutyryl-CoA hydrolase (HIBCH) as a possible toxicity-causing off-target of tolcapone, and this protein is not bound by the less toxic COMT inhibitor entacapone. Moreover, two novel compounds from a focused library synthesized in-house, N(2),N(2),N(3),N(3)-tetraethyl-6,7-dihydroxy-5-nitronaphthalene-2,3-dicarboxamide and 5-(3,4-dihydroxy-5-nitrobenzylidene)-3-ethylthiazolidine-2,4-dione, were utilized to gain insight into the structure-activity relationships in binding to COMT and the novel off-target HIBCH. These compounds, especially N(2),N(2),N(3),N(3)-tetraethyl-6,7-dihydroxy-5-nitronaphthalene-2,3-dicarboxamide, could serve as starting point for the development of improved and more specific COMT inhibitors. PMID:27074629

  5. Laser-induced electron capture mass spectrometry

    Science.gov (United States)

    Wang; Giese

    2000-02-15

    Two techniques are reported for detection of electrophorederivatized compounds by laser-induced electron capture time-of-flight mass spectrometry (LI-EC-TOF-MS). In both cases, a nitrogen laser is used to induce the electron capture. The analyte is deposited in a matrix consisting of a compound with a low ionization potential such as benzo[ghi]perylene in the first technique, where the electron for electron capture apparently comes from this matrix. In the second technique, the analyte is deposited on a silver surface in the absence of matrix. It seems that "monoenergetic" ions instantly desorb from the target surface in the latter case, since the peak width in the continuous extraction mode essentially matches the pulse width of the laser (4 ns). Ten picomoles of 3-O-(pentafluorobenzyl)-alpha-estradiol were detected at a S/N > or = 50, where the spot size of the laser was approximately 0.25% of the sample spot. It is attractive that simple conditions can enable sensitive detection of electrophores on routine TOF-MS equipment. The technique can be anticipated to broaden the range of analytes in both polarity and size that can be detected by EC-MS relative to the range for GC/EC-MS. PMID:10701262

  6. Carbon dioxide capture by means of cyclic organic nitrogen compounds

    OpenAIRE

    García Abuín, Alicia

    2012-01-01

    The research work included in present PhD Thesis involves the research studies to capture carbon dioxide using different cyclic nitrogen organic compounds (glucosamine (GA), chitosan (C), alkyl-pyrrolidones, pyrrolidine (PYR) and piperidine (PIP). This investigation is based on the study of three experimental systems. Each of them has characteristics potentially suitable to achieve the aim of this work, that is to say, to improve the carbon dioxide capture process, which is pre...

  7. Metabolism of halogenated compounds in the white rot fungus Bjerkandera adusta studied by membrane inlet mass spectrometry and tandem mass spectrometry

    DEFF Research Database (Denmark)

    Beck, Hans Christian; Lauritsen, F.R.; Patrick, J.S.;

    1996-01-01

    Membrane inlet mass spectrometry has been used for the characterization of halogenated organic compounds produced by the fungus Bjerkandera adusta. Using this technique, electron impact-, chemical ionization-, electron capture negative chemical ionization-mass spectra and tandem mass spectra were...

  8. Mass spectrometry for determination of bioactive compounds

    Digital Repository Service at National Institute of Oceanography (India)

    Tilvi, S.; Majik, M.S.; Singh, K.S.

    cell. This type of experiment is particularly useful for monitoring groups of compounds contained within a mixture which fragment to produce common fragment ions, e.g. glycosylated peptides in a tryptic digest mixture, aliphatic hydrocarbons in an oil... in a matrix e.g. drug testing with blood or urine samples. It is not only a highly specific method but also has very high sensitivity. For known compounds, mass spectra can be used much like fingerprints. A match is extremely strong evidence...

  9. Photoinduced mass transport in azo compounds

    Science.gov (United States)

    Klismeta, K.; Teteris, J.; Aleksejeva, J.

    2013-12-01

    The photoinduced changes of optical properties in azobenzene containing compound thin films were studied under influence of polarized and non-polarized 532 nm laser light. Under influence of light azo compounds experience trans-cis isomerisation process, that can be observed in the absorbance spectrum of the sample. If the light is linearly polarized, molecules align perpendicularly to the electric field vector and as a result photoinduced dichroism and birefringence is obtained. If a known lateral polarization modulation of the light beam is present, mass transport of the azobenzene containing compound occurs. By measuring the surface relief with a profilometer the direction of mass transport can be determined. The studies of this work show that direct holographic recording of surface relief gratings can be used in optoelectronics, telecommunications and data storage.

  10. Mass spectral investigations of boron neutron capture therapy (BNCT) agents

    International Nuclear Information System (INIS)

    Boron neutron capture therapy (BNCT) is a promising technique for the treatment of selected types of brain tumor and potentially for other tumor types. In this therapy, a 10B-enriched species is administered to the bloodstream and selectively deposited in the tumor. The selective deposition in the tumor is due to either the breakdown of the blood-grain barrier or to the chemical nature of the boron-containing compounds. Once a sufficient concentration of boron is attained in the tumor (approximately 25 ppm), the tumor is irradiated with a controlled energy neutron beam (preferable epithermal, 1 eV to 10 keV), at which time neutrons are captured by the incorporated boron atoms. The capture results in the reaction, 10B(n, ) Li, which produces a localized nuclear reaction capable of destroying the tumor cell containing the boron. A variety of boron containing compounds have been evaluated for use in BNCT. This paper addresses some of the most promising of the compounds, the disodium salt of mercaptoundecahydrododecaborate (Na2B12H11SH), commonly referred to as BSH

  11. New compounds for neutron capture therapy (NCT) and their significance

    International Nuclear Information System (INIS)

    Clearly the most effective tumor therapy would be obtained by the selective targeting of cytotoxic agents to tumor cells. Although many biomolecules are known to be taken up in tumors, the targeting of cytotoxic agents to tumors is limited by the fact that other essential cell pools compete with equal or even greater effectiveness. The approach of delivering stable non-toxic isotopes to tumor, with activation by means of an external radiation beam, is advantageous for two reasons: (1) it obviates problems associated with high uptake of isotopes in normal tissues, as these cell pools can be excluded from the radiation field, and (2) the general tumor area can be included in the activating beam field; thus, the possibility exists that all microscopic tumor extensions can be irradiated. As long as range of reaction products is short, dose will be restricted to the tumor, with a resultant high therapeutic ratio. This method can be accomplished with either photon activation therapy (PAT) or Neutron Capture Therapy (NCT), the latter will be emphasized here. The range of the high LET, low OER particles from the 10B(n,α)7Li reaction is approx. 10 μm, or one cell diameter; hence this reaction is optimal for cell killing. A number of biomolecules have been investigated as possible vehicles for transport of boron to tumors, including phenothiazines, thiouracils, porphyrins, nucleosides, and amino acids. Biodistributions of these compounds show selective concentration in tumor adequate for therapy. The biological halflives are in the order of days, allowing the possibility of fractionated or protracted irradiations. The radiobiological and physical implication of these parameters on NCT are discussed. The possibility of using an approximately-monoenergetic, scandium-filtered beam of about 2 keV, to reduce the dose from background radiations by about 85%, is also discussed

  12. A New Mass Criterium for Electron Capture Supernovae

    Science.gov (United States)

    Poelarends, Arend

    2016-06-01

    Electron capture supernovae (ECSN) are thought to populate the mass range between massive white dwarf progenitors and core collapse supernovae. It is generally believed that the initial stellar mass range for ECSN from single stars is about 0.5-1.0 M⊙ wide and centered around a value of 8.5 or 9 M⊙, depending on the specifics of the physics of convection and mass loss one applies. Since mass loss in a binary system is able to delay or cancel the second dredge-up, it is also believed that the initial mass range for ECSN in binary systems is wider than in single stars, but an initial mass range has not been defined yet.The last phase of stars in this particular mass range, however, is challenging to compute, either due to recurring Helium shell flashes, or due to convectively bound flames in the degenerate interior of the star. It would be helpful, nevertheless, to know before we enter these computationally intensive phases whether a star will explode as an ECSN or not. The mass of the helium core after helium core burning is one such criterium (Nomoto, 1984), which predicts that ECSN will occur if the helium core mass is between 2.0 M⊙ and 2.5 M⊙. However, since helium cores can be subject to erosion due to mass loss — even during helium core burning, this criterium will not yield accurate predictions for stars in binary systems.We present a dense grid of stellar evolution models that allow us to put constraints on the final fate of their cores, based on a combination of Carbon/Oxygen core mass, the mass of the surrounding Helium layer and C/O abundance. We find that CO cores with masses between 1.365 and 1.420 M⊙ at the end of Carbon burning will result in ECSN, with some minor adjustments of these ranges due to the mass of the Helium layer and the C/O ratio. While detailed models of stars within the ECSN mass range remain necessary to understand the details of pre-ECSN evolution, our research refines the Helium core criterion and provides a useful way

  13. Capture and release of acid-gasses with acid-gas binding organic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Heldebrant, David J; Yonker, Clement R; Koech, Phillip K

    2015-03-17

    A system and method for acid-gas capture wherein organic acid-gas capture materials form hetero-atom analogs of alkyl-carbonate when contacted with an acid gas. These organic-acid gas capture materials include combinations of a weak acid and a base, or zwitterionic liquids. This invention allows for reversible acid-gas binding to these organic binding materials thus allowing for the capture and release of one or more acid gases. These acid-gas binding organic compounds can be regenerated to release the captured acid gasses and enable these organic acid-gas binding materials to be reused. This enables transport of the liquid capture compounds and the release of the acid gases from the organic liquid with significant energy savings compared to current aqueous systems.

  14. Improved Actinide Neutron Capture Cross Sections Using Accelerator Mass Spectrometry

    Science.gov (United States)

    Bauder, W.; Pardo, R. C.; Kondev, F. G.; Kondrashev, S.; Nair, C.; Nusair, O.; Palchan, T.; Scott, R.; Seweryniak, D.; Vondrasek, R.; Collon, P.; Paul, M.; Youinou, G.; Salvatores, M.; Palmotti, G.; Berg, J.; Maddock, T.; Imel, G.

    2014-09-01

    The MANTRA (Measurement of Actinide Neutron TRAnsmutations) project will improve energy-integrated neutron capture cross section data across the actinide region. These data are incorporated into nuclear reactor models and are an important piece in understanding Generation IV reactor designs. We will infer the capture cross sections by measuring isotopic ratios from actinide samples, irradiated in the Advanced Test Reactor at INL, with Accelerator Mass Spectrometry (AMS) at ATLAS (ANL). The superior sensitivity of AMS allows us to extract multiple cross sections from a single sample. In order to analyze the large number of samples needed for MANTRA and to meet the goal of extracting multiple cross sections per sample, we have made a number of modifications to the AMS setup at ATLAS. In particular, we are developing a technique to inject solid material into the ECR with laser ablation. With laser ablation, we can better control material injection and potentially increase efficiency in the ECR, thus creating less contamination in the source and reducing cross talk. I will present work on the laser ablation system and preliminary results from our AMS measurements. The MANTRA (Measurement of Actinide Neutron TRAnsmutations) project will improve energy-integrated neutron capture cross section data across the actinide region. These data are incorporated into nuclear reactor models and are an important piece in understanding Generation IV reactor designs. We will infer the capture cross sections by measuring isotopic ratios from actinide samples, irradiated in the Advanced Test Reactor at INL, with Accelerator Mass Spectrometry (AMS) at ATLAS (ANL). The superior sensitivity of AMS allows us to extract multiple cross sections from a single sample. In order to analyze the large number of samples needed for MANTRA and to meet the goal of extracting multiple cross sections per sample, we have made a number of modifications to the AMS setup at ATLAS. In particular, we are

  15. Low Mass Printable Devices for Energy Capture, Storage, and Use

    Science.gov (United States)

    Frazier, Donald O.; Singer, Christopher E.; Rogers, Jan R.; Schramm, Harry F.; Fabisinski, Leo L.; Lowenthal, Mark; Ray, William J.; Fuller, Kirk A.

    2010-01-01

    The energy-efficient, environmentally friendly technology that will be presented is the result of a Space Act Agreement between NthDegree Technologies Worldwide, Inc., and the National Aeronautics and Space Administration's (NASA's) Marshall Space Flight Center (MSFC). The work combines semiconductor and printing technologies to advance lightweight electronic and photonic devices having excellent potential for commercial and exploration applications. Device development involves three projects that relate to energy generation and consumption: (1) a low-mass efficient (low power, low heat emission) micro light-emitting diode (LED) area lighting device; (2) a low-mass omni-directional efficient photovoltaic (PV) device with significantly improved energy capture; and (3) a new approach to building super-capacitors. These three technologies, energy capture, storage, and usage (e.g., lighting), represent a systematic approach for building efficient local micro-grids that are commercially feasible; furthermore, these same technologies, appropriately replacing lighting with lightweight power generation, will be useful for enabling inner planetary missions using smaller launch vehicles and to facilitate surface operations during lunar and planetary surface missions. The PV device model is a two sphere, light trapped sheet approximately 2-mm thick. The model suggests a significant improvement over current thin film systems. For lighting applications, all three technology components are printable in-line by printing sequential layers on a standard screen or flexographic direct impact press using the three-dimensional printing technique (3DFM) patented by NthDegree. One primary contribution to this work in the near term by the MSFC is to test the robustness of prototype devices in the harsh environments that prevail in space and on the lunar surface. It is anticipated that this composite device, of which the lighting component has passed off-gassing testing, will function

  16. Carborane compounds for neutron capture therapy of malignant melanoma

    International Nuclear Information System (INIS)

    The possibility of using thiouracil as a vehicle for stable nuclei such as 10B for neutron capture therapy (NCT) of melanoma was first discussed by Fairchild and co-workers in 1982. The author's research has been directed towards the design and synthesis of a number of o-carboranyl-thiouracils, the ten boron atoms of the carborane cage having a clear advantage for NCT. The first step was the preparation, previously reported, of thiouracils bearing an alkyl group continuing a triple bond for later elaboration to a carborane. The present paper describes the continuation of this work with the preparation of the carboranes of this series and its extension to the synthesis of a thiouracil in which a carboranylalkyl group is attached to the nitrogen in the 3-position

  17. Mass spectrometric analysis of simple hydrogen compounds

    International Nuclear Information System (INIS)

    A uranium furnace is inserted in the gas inlet line of a mass spectrometer between the leak and the source. The line is fed with simple hydrogen compounds (H2O, NH3, H2S) which are in this way reduced to hydrogen gas. Memory effects are largely avoided by heating the sample line to 90 deg. C. The speed of the isotopic analysis is only slightly less than that of hydrogen gas itself; the accuracy is better due to the reduction of fractionating effects in the leak. For the absolute measurements of deuterium in water, the presence of H3+ is a problem. Water samples, prepared by mixing an unknown light water sample with different amounts of heavy water, are equilibrated with hydrogen sulphide and analysis of the two phases of each sample enables the zero of the concentration scale to be determined from the point of intersection of the two curves obtained by plotting mixture composition against the observed isotope ratio in the two phases. The whole experiment can be carried out in the apparatus described which analyses hydrogen in H2S and H2O in the same way. (author)

  18. Ratio variation of electron capture probability to positron decay probability for 68Ga in chemical compounds

    International Nuclear Information System (INIS)

    The change of 68 Ga gamma-line intensities in different chemical compounds is studied.Electron capture (EC) competes with 68 Ga β+ decay. The effect of chemical environment on the probabilities of these processes is different. Radioactive sources are prepared in the form of GeS and GeO2 compounds with 68 Ge (T1/2=288 days; the decay is due to EC with 68Ga formation in the ground state). The measured value of intensity change δI/I for 68 Ga in GeS relative to GeO equals (11+-3)x10-4

  19. A new route for neutrino mass determination using the electron capture of {sup 194}Hg

    Energy Technology Data Exchange (ETDEWEB)

    Beck, Dietrich; Herfurth, Frank [GSI, Darmstadt (Germany); Blaum, Klaus; Boehm, Christine [MPI fuer Kernphysik, Heidelberg (Germany); Ruprecht-Karls-Universitaet, Heidelberg (Germany); Breitenfeldt, Martin; Schweikhard, Lutz [Ernst-Moritz-Arndt-Universitaet, Greifswald (Germany); Eliseev, Sergey; George, Sebastian [MPI fuer Kernphysik, Heidelberg (Germany); Fedosseev, Valentin; Herlert, Alexander; Kowalska, Magdalena; Seliverstov, Maxim [CERN, Geneve (Switzerland); Lunney, David; Naimi, Sarah [Universite de Paris Sud, Orsay (France); Neidherr, Dennis [Johannes Gutenberg-Universitaet, Mainz (Germany); Novikov, Yuri [PNPI, Gatchina, St. Petersburg (Russian Federation); Schwarz, Stefan [NSCL, MSU, East Lansing, Michigan (United States); Zuber, Kai [Technische Universitaet, Dresden (Germany)

    2010-07-01

    The electron neutrino mass is of highest importance for many fields of physics. To measure the neutrino mass, beta-decay spectra are typically used. Here an alternative way to determine the neutrino mass, using an electron capture in {sup 194}Hg will be presented. Direct mass measurements of {sup 194}Hg and its daughter nucleus {sup 194}Au were performed at the high-precision Penning trap mass spectrometer ISOLTRAP at the ISOLDE facility (CERN). The Q{sub EC}-value obtained by the mass difference of these nuclei leads to the conclusion that the K-capture is forbidden, thus an L-capture is assumed. For further investigations a measurement using a cryogenic micro-calorimeter is suggested. From this, a de-excitation spectrum is obtained which can be compared to the Q{sub EC}-value in order to determine the neutrino mass.

  20. Low Mass Printable Devices for Energy Capture, Storage, and Use for Space Exploration Missions

    Science.gov (United States)

    Frazier, Donald O.; Singer, Christopher E.; Ray, William J.; Fuller, Kirk A.

    2010-01-01

    The energy-efficient, environmentally friendly technology that will be presented is the result of a Space Act Agreement between -Technologies Worldwide, Inc., and the National Aeronautics and Space Administration s (NASA s) Marshall Space Flight Center (MSFC). This work combines semiconductor and printing technologies to advance lightweight electronic and photonic devices having excellent potential for commercial and exploration applications, and is an example of industry and government cooperation that leads to novel inventions. Device development involves three energy generation and consumption projects: 1) a low mass efficient (low power, low heat emission) micro light-emitting diode (LED) area lighting device; 2) a low-mass omni-directional efficient photovoltaic (PV) device with significantly improved energy capture; and 3) a new approach to building supercapacitors. These three technologies - energy capture, storage, and usage (e.g., lighting) - represent a systematic approach for building efficient local micro-grids that are commercially feasible; furthermore, these same technologies will be useful for lightweight power generation that enables inner planetary missions using smaller launch vehicles and facilitates surface operations. The PV device model is a two-sphere, light-trapped sheet approximately 2-mm thick. The model suggests a significant improvement over current thin film systems. All three components may be printed in line by printing sequential layers on a standard screen or flexographic direct impact press using the threedimensional printing technique (3DFM) patented by NthDegree. MSFC is testing the robustness of prototype devices in the harsh space and lunar surface environments, and available results will be reported. Unlike many traditional light sources, this device does not contain toxic compounds, and the LED component has passed stringent off-gassing tests required for potential manifesting on spacecraft such as the International Space

  1. Neutrino mass, neutrinoless double electron capture and rare beta decays

    Energy Technology Data Exchange (ETDEWEB)

    Mustonen, M T; Suhonen, J, E-mail: jouni.suhonen@phys.jyu.f [Department of Physics, PO Box 35 (YFL), FI-40014 University of Jyvaeskylae (Finland)

    2010-01-01

    We present results of our theoretical calculations on three nuclei of interest from the neutrino-physics point of view: Firstly, we present the second-forbidden decay branch of {sup 115}In with the ultra-low Q value and theoretical open questions related to such decays. Secondly, we have calculated estimates for the half-lives of the single-beta decay channels of {sup 96}Zr and concluded that the possible contamination from those to the geochemical measurements of {sup 96}Zr double-beta-decay half-life is rather small. Thirdly, we have taken a look at the neutrinoless resonance double-electron-capture decay of {sup 112}Sn in the light of recent JYFLTRAP Q value measurements and discovered that the badly fulfilled resonance condition renders the decay unobservable.

  2. Search for new candidates for the neutrino-oriented mass determination by electron-capture

    CERN Multimedia

    Herfurth, F; Boehm, C; Blaum, K; Beck, D

    2008-01-01

    This proposal is part of an extended program dedicated to the neutrino-mass determination in the electron-capture sector, which aims at ultra-precise mass measurements by Penning traps in combination with cryogenic micro-calorimetry for atomic de-excitation measurements. Here, precise mass measurements with ISOLTRAP are proposed for the orbital electron-capture nuclides $^{194}$Hg and $^{202}$Pb, as well as their daughters, with the goal to determine accurately their Q-values. These values are expected to be the smallest ones among a great variety of known electron-capture precursors. Therefore, these nuclides are strong candidates for an improved electron-neutrino mass determination. We ask for 8 shifts of on-line beam at ISOLDE for mass measurements of $^{194}$Hg, $^{194}$ Au, $^{202}$Pb, and $^{202}$Tl at ISOLTRAP.

  3. Boron-Containing Compounds for Liposome-Mediated Tumor Localization and Application to Neutron Capture Therapy

    International Nuclear Information System (INIS)

    Medical application of boron neutron capture therapy (BNCT) has been significantly hindered by the slow development of boron drug-targeting methodologies for the selective delivery of high boron concentration sto malignant cells. We have successfully sought to fill this need by creating liposomes suitable as in vivo boron delivery vehicles for BNCT. Delivery of therapeutic quantities of boron to tumors in murine models has been achieved with small unilamellar boron-rich liposomes. Subsequently, attempts have been made to improve delivery efficiency of liposomes encapsulating boron-containing water-soluble species into their hollow core by incorporating lipophilic boron compounds as addenda to the liposome bilayer, incorporating boron compounds as structural components of the bilayer (which however, poses the risk of sacrificing some stability), and combinations thereof. Regardless of the method, approximately 90% of the total liposome mass remains therapeutically inactive and comprised of the vehicle's construction materials, while less than 5% is boron for neutron targeting. Following this laboratory's intensive study, the observed tumor specificity of certain liposomes has been attributed to their diminutive size of these liposomes (30-150 nm), which enables these small vesicles to pass through the porous, immature vasculature of rapidly growing tumor tissue. We surmised that any amphiphilic nanoparticle of suitable size could possess some tumor selectivity. Consequently, the discovery of a very boron-rich nanoparticle delivery agent with biodistribution performance similar to unilamellar liposomes became one of our goals. Closomers, a new class of polyhedral borane derivatives, attracted us as an alternative BNCT drug-delivery system. We specifically envisioned dodeca (nido-carboranyl)-substituted closomers as possibly having a great potential role in BNCT drug delivery. They could function as extraordinarily boron-rich BNCT drugs since they are amphiphilic

  4. Boron-Containing Compounds for Liposome-Mediated Tumor Localization and Application to Neutron Capture Therapy

    Energy Technology Data Exchange (ETDEWEB)

    Hawthorne, M. Frederick [Univ. of California, Los Angeles, CA (United States)

    2005-04-07

    Medical application of boron neutron capture therapy (BNCT) has been significantly hindered by the slow development of boron drug-targeting methodologies for the selective delivery of high boron concentration sto malignant cells. We have successfully sought to fill this need by creating liposomes suitable as in vivo boron delivery vehicles for BNCT. Delivery of therapeutic quantities of boron to tumors in murine models has been achieved with small unilamellar boron-rich liposomes. Subsequently, attempts have been made to improve delivery efficiency of liposomes encapsulating boron-containing water-soluble species into their hollow core by incorporating lipophilic boron compounds as addenda to the liposome bilayer, incorporating boron compounds as structural components of the bilayer (which however, poses the risk of sacrificing some stability), and combinations thereof. Regardless of the method, approximately 90% of the total liposome mass remains therapeutically inactive and comprised of the vehicle's construction materials, while less than 5% is boron for neutron targeting. Following this laboratory's intensive study, the observed tumor specificity of certain liposomes has been attributed to their diminutive size of these liposomes (30-150 nm), which enables these small vesicles to pass through the porous, immature vasculature of rapidly growing tumor tissue. We surmised that any amphiphilic nanoparticle of suitable size could possess some tumor selectivity. Consequently, the discovery of a very boron-rich nanoparticle delivery agent with biodistribution performance similar to unilamellar liposomes became one of our goals. Closomers, a new class of polyhedral borane derivatives, attracted us as an alternative BNCT drug-delivery system. We specifically envisioned dodeca (nido-carboranyl)-substituted closomers as possibly having a great potential role in BNCT drug delivery. They could function as extraordinarily boron-rich BNCT drugs since they are

  5. Cure of malignant melanoma by single thermal neutron capture treatment using melanoma-seeking compounds

    International Nuclear Information System (INIS)

    Since not only malignant melanomas but also many kinds of human cancers, for example thyroid cancer and squamous cell carcinoma, synthesize their specific protein, much attention has been paid to the establishment of selective thermal neutron capture treatment of malignant melanoma as a prototype of such cancer cells. This paper presents 10B chlorpromazine compounds and 10B1-para-boronophenylalanine (10B1-BPA) as tumor-seeking 10B compounds which themselves possess selective affinity for the specific metabolic activity of the target cancer cells. An overview of the following studies on the effects of 10B1-BPA in the thermal neutron capture treatment of melanoma is provided: 1) in vitro studies on specific enhanced melanoma cell killing effects of 10B1-BPA; 2) in vivo studies on therapeutic effects of 10B1-BPA using melanoma-bearing hamsters; and 3) preclinical therapeutic experiments using spontaneously occurring malignant melanoma in Duroc pig skin, including experiments in which melanoma was successfully cured. (Namekawa, K.)

  6. The volatile compound BinBase mass spectral database

    Directory of Open Access Journals (Sweden)

    Barupal Dinesh K

    2011-08-01

    Full Text Available Abstract Background Volatile compounds comprise diverse chemical groups with wide-ranging sources and functions. These compounds originate from major pathways of secondary metabolism in many organisms and play essential roles in chemical ecology in both plant and animal kingdoms. In past decades, sampling methods and instrumentation for the analysis of complex volatile mixtures have improved; however, design and implementation of database tools to process and store the complex datasets have lagged behind. Description The volatile compound BinBase (vocBinBase is an automated peak annotation and database system developed for the analysis of GC-TOF-MS data derived from complex volatile mixtures. The vocBinBase DB is an extension of the previously reported metabolite BinBase software developed to track and identify derivatized metabolites. The BinBase algorithm uses deconvoluted spectra and peak metadata (retention index, unique ion, spectral similarity, peak signal-to-noise ratio, and peak purity from the Leco ChromaTOF software, and annotates peaks using a multi-tiered filtering system with stringent thresholds. The vocBinBase algorithm assigns the identity of compounds existing in the database. Volatile compound assignments are supported by the Adams mass spectral-retention index library, which contains over 2,000 plant-derived volatile compounds. Novel molecules that are not found within vocBinBase are automatically added using strict mass spectral and experimental criteria. Users obtain fully annotated data sheets with quantitative information for all volatile compounds for studies that may consist of thousands of chromatograms. The vocBinBase database may also be queried across different studies, comprising currently 1,537 unique mass spectra generated from 1.7 million deconvoluted mass spectra of 3,435 samples (18 species. Mass spectra with retention indices and volatile profiles are available as free download under the CC-BY agreement (http

  7. Oscillating Decay Rate in Electron Capture and the Neutrino Mass Difference

    CERN Document Server

    Peshkin, Murray

    2014-01-01

    Reported oscillations in the rate of decay of certain ions by K-electron capture have raised questions about whether and how such oscillations can arise in quantum mechanical theory and whether they can measure the neutrino mass difference. Here I show that simple principles of quantum mechanics answer some questions and clarify what must be done theoretically or experimentally to answer some others.

  8. Analysis of organosulfur compounds in produced waters using mass spectrometry

    International Nuclear Information System (INIS)

    Produced water is a complex waste effluent generated during offshore oil production. The recent efforts are aimed at providing information that can be used to assess the effects of produced water discharges into the coastal environment near Gaviota, California. Analysis of dichloromethane extracts of produced water samples revealed that a series of polar organosulfur compounds of intermediate polarity are abundant constituents. A suite of mass spectrometric techniques including electron ionization, chemical ionization, high resolution mass spectrometry, and MS/MS are being used for chemical characterization. These chemicals are present in far greater concentrations than petroleum hydrocarbons in the same waste stream, but the environmental importance and the origins of these compounds remain unclear. Studies are underway using model compounds to test the hypothesis that they arise from reactions of abundant sulfides with other organic compounds. Assessment of the distribution of produced water constituents near the discharge outfall is being performed by sampling seawater, mussels, and sediment at two depths at three sites in the vicinity of the outfall. The authors have developed analytical protocols for determination of organosulfur constituents in each of these matrices. Simultaneous analysis of lipid profiles from the mussels can be carried out without modification of the analytical procedures

  9. The Role of Electron Captures in Chandrasekhar Mass Models for Type Ia Supernovae

    CERN Document Server

    Brachwitz, F; Hix, W R; Iwamoto, K; Langanke, K; Martínez-Pinedo, G; Nomoto, K; Strayer, M R; Thielemann, F K; Umeda, H; Brachwitz, Franziska; Dean, David J.; Iwamoto, Koichi; Langanke, Karlheinz; Martinez-Pinedo, Gabriel; Nomoto, Ken'ichi; Strayer, Michael R.; Thielemann, Friedrich-K.; Umeda, Hideyuki

    2000-01-01

    The Chandrasekhar mass model for Type Ia Supernovae (SNe Ia) has received increasing support from recent comparisons of observations with light curve predictions and modeling of synthetic spectra. It explains SN Ia events via thermonuclear explosions of accreting white dwarfs in binary stellar systems, being caused by central carbon ignition when the white dwarf approaches the Chandrasekhar mass. As the electron gas in white dwarfs is degenerate, characterized by high Fermi energies for the high density regions in the center, electron capture on intermediate mass and Fe-group nuclei plays an important role in explosive burning. Electron capture affects the central electron fraction Y_e, which determines the composition of the ejecta from such explosions. Up to the present, astrophysical tabulations based on shell model matrix elements were only available for light nuclei in the sd-shell. Recently new Shell Model Monte Carlo (SMMC) and large-scale shell model diagonalization calculations have also been perform...

  10. Can neutrino mass be measured in low-energy electron capture decay?

    CERN Document Server

    Robertson, R G H

    2014-01-01

    The standard kinematic method for determining neutrino mass from the beta decay of tritium or other isotope is to measure the shape of the electron spectrum near the endpoint. It has been known for 30 years that a similar distortion of the "visible energy" remaining after electron capture is caused by neutrino mass. There has been a resurgence of interest in using this method with 163-Ho. Recent theoretical analyses offer reassurance that there are no significant theoretical uncertainties. We show that the situation is, however, more complicated, and that the spectrum shape is presently not well enough understood to permit a sensitive determination of the neutrino mass in this way.

  11. Radiative proton capture cross sections in the mass range 40-54

    Science.gov (United States)

    Chakraborty, Dipti; Dutta, Saumi; Gangopadhyay, G.; Bhattacharyya, Abhijit

    2016-07-01

    Proton capture cross sections in the energy range of astrophysical interest for mass region 40-54 have been calculated in the Hauser-Feshbach formalism with the reaction code talys1.6. The density-dependent M3Y effective nucleon-nucleon interaction folded with target radial matter densities from the relativistic mean field approach is used to obtain the semimicroscopic optical potential. A definite normalization of potential well depths has been used over the entire mass region. The (p ,γ ) rates of some reactions, important in the astrophysical scenario, are calculated using the potential in the relevant mass region.

  12. Radiative proton capture cross sections in the mass range $40-55$

    CERN Document Server

    Chakraborty, Dipti; Gangopadhyay, G; Bhattacharyya, Abhijit

    2016-01-01

    Proton capture cross sections in the energy range of astrophysical interest for mass region 40-54 have been calculated in the Hauser-Feshbach formalism with reaction code TALYS1.6. The density dependent M3Y effective nucleon-nucleon interaction folded with target radial matter densities from relativistic mean field approach is used to obtain the semi-microscopic optical potential. A definite normalization of potential-well depths has been used over the entire mass region. The $(p,\\gamma)$ rates of some reactions, important in the astrophysical scenario, are calculated using the potential in the relevant mass region.

  13. For boron neutron capture therapy,synthesizing boron-polymer compounds and testing in laboratory conditions

    International Nuclear Information System (INIS)

    The aim of this project is to establish a focus point at Turkish Atomic Energy Authority (TAEA) in the field of Boron Neutron Capture Therapy which is a binary radiotherapy method for brain tumours. Moreover in the scope of the project, a new alternative of 10B-carrier compounds will be synthesized, the neutron source will be determined and the infrastructure to start the clinical trials of BNCT in our country will be established. BNCT is a binary radiotherapy method and the successful of this method is depend on the synthesized boron compounds which have the selective targeting property with tumour cells and neutron optimization. The water-soluble polymer based boron compounds having biochemical and physiological properties will be synthesized and cell culture experiment will be done. In addition, after the neutron source is set up in our country, the infrastructure studies will be started in order to start the clinical trials of BNCT. In this project, there are three different groups as boron compounds, neutron physics and medical group. Neutron physics group is starting the calculations of neutron beam parameters using in BNCT application. But, medical group has no active studies yet. Boron compounds group has been carried out two different experimental studies. In the first experimental study, functional groups have been bound to boron containing polymers to enhance the selectively targeting property and characterized by various analysis methods. Later, cell culture experiment will be done. The first study has been carried out with Hacettepe University. Up to present, completed studies are listed as: -Maleic anhydride oligomer was synthesized and then 2-aminoethyl diphenyl borate (2-AEPB) and monomethoxy poly(ethylene glycol) (PEG) was bound to this oligomer, respectively. Thus, [MAH]n-g1-2-AEPB-g2-PEG was synthesized. -2-AEPB compound were bound to poly(acrylic acid) polymer at different three mole ratio.Then, the selected Poli(Ac)-g1-2-AEPB polymer was

  14. Determination of high molecular mass compounds from Amazonian plant's leaves

    International Nuclear Information System (INIS)

    The fractions of dichloromethane extracts of leaves from andiroba (Carapa guianensis - Meliaceae), caapi (Banisteriopsis caapi - Malpighiaceae), cocoa (Theobroma cacao - Sterculiaceae), Brazil nut (Bertholletia excelsa - Lecytidaceae), cupuacu (Theobroma grandiflorum - Sterculiaceae), marupa (Simaruba amara - Simaroubaceae) and rubber tree (Hevea brasiliensis - Euphorbiaceae), were analyzed by HT-HRGC and HT-HRGC-MS. Esters of homologous series of fatty acids and long chain alcohols, phytol, amyrines and tocopherols were characterized. The characterization of the compounds was based mainly in mass spectra data and in addition by usual spectrometric data (1H and 13C NMR, IR). (author)

  15. Pressure Drop, Capacity and Mass Transfer Area Requirements for Post-Combustion Carbon Capture by Solvents

    International Nuclear Information System (INIS)

    Post-combustion capture processes using amines are considered as one of the preferred options for CO2 Capture and Storage (CCS). However, the cost of avoided CO2 is very large and must be reduced. The latter cost is strongly linked with column designs which consequently must be optimized. In the present article, hydrodynamics and mass transfer performances of random and structured packings are discussed in terms of pressure drop, capacity and most importantly in terms of mass transfer parameters, in particular in terms of interfacial area which is the most important parameter for CO2 absorbers design. Comparison of different commercial high efficiency packings is discussed from experimental characterization and from CFD simulations and a methodology for future developments is proposed. (authors)

  16. Determining the Binding Sites of β-Cyclodextrin and Peptides by Electron-Capture Dissociation High Resolution Tandem Mass Spectrometry

    Science.gov (United States)

    Qi, Yulin; Geib, Timon; Volmer, Dietrich A.

    2015-07-01

    Cyclodextrins (CDs) are a group of cyclic oligosaccharides, which readily form inclusion complexes with hydrophobic compounds to increase bioavailability, thus making CDs ideal drug excipients. Recent studies have also shown that CDs exhibit a wide range of protective effects, preventing proteins from aggregation, degradation, and folding. These effects strongly depend on the binding sites on the protein surface. CDs only exhibit weak interactions with amino acids, however; conventional analytical techniques therefore usually fail to reveal the exact location of the binding sites. Moreover, some studies even suggest that CD inclusion complexes are merely electrostatic adducts. Here, electron capture dissociation (ECD) was applied in this proof-of-concept study to examine the exact nature of the CD/peptide complexes, and CD binding sites were unambiguously located for the first time via Fourier-transform ion cyclotron resonance (FTICR) tandem mass spectrometry.

  17. The Role of Electron Captures in Chandrasekhar-Mass Models for Type Ia Supernovae

    International Nuclear Information System (INIS)

    The Chandrasekhar-mass model for Type Ia supernovae (SNe Ia) has received increasing support from recent comparisons of observations with light-curve predictions and modeling of synthetic spectra. It explains SN Ia events via thermonuclear explosions of accreting white dwarfs in binary stellar systems, being caused by central carbon ignition when the white dwarf approaches the Chandrasekhar mass. As the electron gas in white dwarfs is degenerate, characterized by high Fermi energies for the high-density regions in the center, electron capture on intermediate-mass and Fe group nuclei plays an important role in explosive burning. Electron capture affects the central electron fraction Ye, which determines the composition of the ejecta from such explosions. Up to the present, astrophysical tabulations based on shell model matrix elements were available only for light nuclei in the sd-shell. Recently, new shell model Monte Carlo and large-scale shell model diagonalization calculations have also been performed for pf-shell nuclei. These lead in general to a reduction of electron capture rates in comparison with previous, more phenomenological, approaches. Making use of these new shell model-based rates, we present the first results for the composition of Fe group nuclei produced in the central regions of SNe Ia and possible changes in the constraints on model parameters like ignition densities ρign and burning front speeds vdef. (c) 2000 The American Astronomical Society

  18. Meson exchange second class currents and the neutrino mass in the muon capture by light nuclei

    International Nuclear Information System (INIS)

    Influence of the Kubodera-Delorme-Rho model parameters (ζ and ξ), the scalar form factor (Fs) and the muonic neutrino rest mass (mνμ) on the asymmetry coefficient (αμν) of neutrino emission with respect to the muon spin orientation in the muon capture by light nuclei is analyzed. It is shown, that the mass mνμ, the parameters of ζ and ξ, and the form factor Fs may be estimated by studying the coefficient αμν in O -> O, Gamov-Teller, and mixed transitions, respectively

  19. Analysis of organic compounds by secondary neutral mass spectrometry (SNMS) and secondary ion mass spectrometry (SIMS)

    International Nuclear Information System (INIS)

    This study is about the use of secondary neutral mass spectrometry (SNMS) and secondary ion mass spectrometry (SIMS) as analytical techniques with depth resolution in determining organic components in environmental solid microparticles. The first application of plasma SNMS to organic compounds revealed the spectra to be composed mainly of signals from the atoms of all participating elements, such as C, H, O, N, S, P, and Cl. In addition, signals produced by multi-atomic clusters can be detected, such as CH, C2, CH2, C2H, and C3, as well as signals indicating the presence of organic compounds with hetero elements, such as OH, NH, and CN. Their intensity decreases very markedly with increasing numbers of atoms. Among the signals from bi-atomic clusters, those coming from elements with large mass differences are most intense. The use of plasma SNMS with organic compounds has shown that, except for spurious chemical reactions induced by ion bombardment and photodesorption by the photons of the plasma, it is possible to analyze with resolution in depth, elements of organic solids. A more detailed molecular characterization of organic compounds is possible by means of SIMS on the basis of multi-atomic fragments and by comparison with suitable signal patterns. (orig./BBR)

  20. Flexible metal-organic framework compounds: In situ studies for selective CO{sub 2} capture

    Energy Technology Data Exchange (ETDEWEB)

    Allen, A.J., E-mail: andrew.allen@nist.gov [Material Measurement Laboratory, National Institute of Standards and Technology (NIST), Gaithersburg, MD 20899-8520 (United States); Espinal, L.; Wong-Ng, W. [Material Measurement Laboratory, National Institute of Standards and Technology (NIST), Gaithersburg, MD 20899-8520 (United States); Queen, W.L. [NIST Center for Neutron Research, Gaithersburg, MD 20899-6102 (United States); The Molecular Foundry, Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA 94720 (United States); Brown, C.M. [NIST Center for Neutron Research, Gaithersburg, MD 20899-6102 (United States); Department of Chemical and Biomolecular Engineering, University of Delaware, Newark, DE 19716 (United States); Kline, S.R. [NIST Center for Neutron Research, Gaithersburg, MD 20899-6102 (United States); Kauffman, K.L. [National Energy Technology Laboratory (NETL), US Department of Energy, Pittsburgh, PA 15236 (United States); Culp, J.T. [National Energy Technology Laboratory (NETL), US Department of Energy, Pittsburgh, PA 15236 (United States); URS Corporation, South Park, PA 15219 (United States); Matranga, C. [National Energy Technology Laboratory (NETL), US Department of Energy, Pittsburgh, PA 15236 (United States)

    2015-10-25

    Results are presented that explore the dynamic structural changes occurring in two highly flexible nanocrystalline metal-organic framework (MOF) compounds during the adsorption and desorption of pure gases and binary mixtures. The Ni(1,2-bis(4-pyridyl)ethylene)[Ni(CN){sub 4}] and catena-bis(dibenzoylmethanato)-(4,4′-bipyridyl)nickel(II) chosen for this study are 3-D and 1-D porous coordination polymers (PCP) with a similar gate opening pressure response for CO{sub 2} isotherms at 303 K, but with differing degrees of flexibility for structural change to accommodate guest molecules. As such, they serve as a potential model system for evaluating the complex kinetics associated with dynamic structure changes occurring in response to gas adsorption in flexible MOF systems. Insights into the crystallographic changes occurring as the MOF pore structure expands and contracts in response to interactions with CO{sub 2}, N{sub 2}, and CO{sub 2}/N{sub 2} mixtures have been obtained from in situ small-angle neutron scattering and neutron diffraction, combined with ex situ X-ray diffraction structure measurements. The role of structure in carbon capture functionality is discussed with reference to the ongoing characterization challenges and a possible materials-by-design approach. - Graphical abstract: We present in situ small-angle neutron scattering results for two flexible metal-organic frameworks (MOFs). The figure shows that for one (NiBpene, high CO{sub 2} adsorption) the intensity of the Bragg peak for the expandable d-spacing most associated with CO{sub 2} adsorption varies approximately with the isotherm, while for the other (NiDBM-Bpy, high CO{sub 2} selectivity) the d-spacing, itself, varies with the isotherm. The cartoons show the proposed modes of structural change. - Highlights: • Dynamic structures of two flexible MOF CO{sub 2} sorbent compounds are compared in situ. • These porous solid sorbents serve as models for pure & dual gas adsorption. • Different

  1. Flexible metal-organic framework compounds: In situ studies for selective CO2 capture

    International Nuclear Information System (INIS)

    Results are presented that explore the dynamic structural changes occurring in two highly flexible nanocrystalline metal-organic framework (MOF) compounds during the adsorption and desorption of pure gases and binary mixtures. The Ni(1,2-bis(4-pyridyl)ethylene)[Ni(CN)4] and catena-bis(dibenzoylmethanato)-(4,4′-bipyridyl)nickel(II) chosen for this study are 3-D and 1-D porous coordination polymers (PCP) with a similar gate opening pressure response for CO2 isotherms at 303 K, but with differing degrees of flexibility for structural change to accommodate guest molecules. As such, they serve as a potential model system for evaluating the complex kinetics associated with dynamic structure changes occurring in response to gas adsorption in flexible MOF systems. Insights into the crystallographic changes occurring as the MOF pore structure expands and contracts in response to interactions with CO2, N2, and CO2/N2 mixtures have been obtained from in situ small-angle neutron scattering and neutron diffraction, combined with ex situ X-ray diffraction structure measurements. The role of structure in carbon capture functionality is discussed with reference to the ongoing characterization challenges and a possible materials-by-design approach. - Graphical abstract: We present in situ small-angle neutron scattering results for two flexible metal-organic frameworks (MOFs). The figure shows that for one (NiBpene, high CO2 adsorption) the intensity of the Bragg peak for the expandable d-spacing most associated with CO2 adsorption varies approximately with the isotherm, while for the other (NiDBM-Bpy, high CO2 selectivity) the d-spacing, itself, varies with the isotherm. The cartoons show the proposed modes of structural change. - Highlights: • Dynamic structures of two flexible MOF CO2 sorbent compounds are compared in situ. • These porous solid sorbents serve as models for pure & dual gas adsorption. • Different degrees of structural freedom give different CO2 adsorption

  2. Electron Capture in 163Ho and Overlap plus Exchange Corrections and the Neutrino Mass

    CERN Document Server

    Faessler, Amand; Simkovic, M F

    2014-01-01

    Holmium offers perhaps the best chance to determine the neutrino mass by electron capture. This contribution treats the electron capture in 163Holmium completely relativistic for the overlap and exchange corrections. The theoretical expressions are derived consistently in second quantisation with the help of Wick's theorem assuming single Slater determinants for the initial Ho and the final Dy atoms with holes in the final ns1/2 and np1/2 states. No hand waving arguments are needed to derive the exchange terms. It seems, that for the first time the multiplicity of electrons in the orbital overlaps are included in the numerical treatment. Electron capture e + p --> n + neutrino is proportional to the probability to find the captured electron in the parent atom at the nucleus. Non-relativistically this is only possible for ns1/2 electron states. Relativistically also p1/2 electrons have a probability to be at the nucleus due to the lower part of the relativistic electron spinor, which does not disappear at the ...

  3. Intratumor heterogeneous distribution of neutron capture compounds suggested by the radiobiological findings concerning sensitivity, repair, reoxygenation and recruitment following neutron capture reaction

    Energy Technology Data Exchange (ETDEWEB)

    Masunaga, Shin-ichiro [Kyoto Univ., Kumatori, Osaka (Japan). Research Reactor Inst

    2000-10-01

    There are many quiescent cells (Q cells) in human solid tumor in comparison with an experimental animal tumor. The control of the Q cells by irradiation is more difficult than the control of proliferous cells (P cells). Recurrence of solid tumor after irradiation therapy is considered as that the uncontrolled Q cells by irradiation proliferate again. One of the most important issues in tumor therapy is to develop a method which destroys effectively the Q cells in solid tumors. Subcutaneous injection of BrdU into mice transplanted SCCV II tumor is carried out in order to mark all of the proliferous cells during 5 days. Neutron capture compound, sodium borocaptate{sup -10}B (BSH) 125 mg/kg, or dl-p-boronophenylalanine-{sup 10}B(BPA) 1500 mg/kg is dosed to the mice. For a series of tests which include sensitivity, potentially lethal damage repair (PLDR), reoxygenation and recruitment of the tumor cells, the mice are irradiated by thermal neutron and gamma-ray with various absorbed doses. The results show that the neutron capture compound concentration in the Q cells, particularly BPA is lower than the concentration in total intratumor cells (P+Q cells). The sensitivity of the Q cells is lower than the P+Q cells, and the PLDR capacity of the Q cells is larger than the P+Q cells. (Suetake, M.)

  4. Comparative Analysis of Mass Spectral Matching-based Compound Identification in Gas Chromatography Mass Spectrometry

    OpenAIRE

    KOO, IMHOI; Kim, Seongho; Zhang, Xiang

    2013-01-01

    Compound identification in gas chromatography–mass spectrometry (GC-MS) is usually achieved by matching query spectra to spectra present in a reference library. Although several spectral similarity measures have been developed and compared using a small reference library, it still remains unknown how the relationship between the spectral similarity measure and the size of reference library affects on the identification accuracy as well as the optimal weight factor. We used three reference lib...

  5. Fully Automated Laser Ablation Liquid Capture Sample Analysis using NanoElectrospray Ionization Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lorenz, Matthias [ORNL; Ovchinnikova, Olga S [ORNL; Van Berkel, Gary J [ORNL

    2014-01-01

    RATIONALE: Laser ablation provides for the possibility of sampling a large variety of surfaces with high spatial resolution. This type of sampling when employed in conjunction with liquid capture followed by nanoelectrospray ionization provides the opportunity for sensitive and prolonged interrogation of samples by mass spectrometry as well as the ability to analyze surfaces not amenable to direct liquid extraction. METHODS: A fully automated, reflection geometry, laser ablation liquid capture spot sampling system was achieved by incorporating appropriate laser fiber optics and a focusing lens into a commercially available, liquid extraction surface analysis (LESA ) ready Advion TriVersa NanoMate system. RESULTS: Under optimized conditions about 10% of laser ablated material could be captured in a droplet positioned vertically over the ablation region using the NanoMate robot controlled pipette. The sampling spot size area with this laser ablation liquid capture surface analysis (LA/LCSA) mode of operation (typically about 120 m x 160 m) was approximately 50 times smaller than that achievable by direct liquid extraction using LESA (ca. 1 mm diameter liquid extraction spot). The set-up was successfully applied for the analysis of ink on glass and paper as well as the endogenous components in Alstroemeria Yellow King flower petals. In a second mode of operation with a comparable sampling spot size, termed laser ablation/LESA , the laser system was used to drill through, penetrate, or otherwise expose material beneath a solvent resistant surface. Once drilled, LESA was effective in sampling soluble material exposed at that location on the surface. CONCLUSIONS: Incorporating the capability for different laser ablation liquid capture spot sampling modes of operation into a LESA ready Advion TriVersa NanoMate enhanced the spot sampling spatial resolution of this device and broadened the surface types amenable to analysis to include absorbent and solvent resistant

  6. Determination of the Electron Neutrino Mass from Experiments on Electron-Capture Beta-Decay (EC)

    CERN Multimedia

    2002-01-01

    The aim of the programme is to measure the electron-neutrino mass, for which at present an upper limit of 500~eV is known. \\\\ \\\\ The experiment studies the shape of the internal bremsstrahlung spectrum in electron-capture near its upper end-point and deduces a mass from small shape changes completely analogous to those in the well-known determination of the electron antineutrino mass in the tritium beta-minus decay. \\\\ \\\\ In a low-energy bremsstrahlung process, the capture takes place from a virtual S state associated with a radiative P~@A~S electromagnetic transition, and the resonant nature of the process leads to important enhancements of the photon intensities at low energy, in particular near the resonance energies co (X-rays). This effect gives this type of experiment a chance to compete with experiments on continuous beta spectra. \\\\ \\\\ The programme concentrates on two long-lived isotopes: \\\\ \\\\ 1)~~|1|6|3Ho. The Q value for this isotope has been found to be 2.6-2.7 keV. A detector specially construct...

  7. Level-resolved quantum statistical theory of electron capture into many-electron compound resonances in highly charged ions

    CERN Document Server

    Berengut, J C; Dzuba, V A; Flambaum, V V; Gribakin, G F

    2015-01-01

    The strong mixing of many-electron basis states in excited atoms and ions with open $f$ shells results in very large numbers of complex, chaotic eigenstates that cannot be computed to any degree of accuracy. Describing the processes which involve such states requires the use of a statistical theory. Electron capture into these 'compound resonances' leads to electron-ion recombination rates that are orders of magnitude greater than those of direct, radiative recombination, and cannot be described by standard theories of dielectronic recombination. Previous statistical theories considered this as a two-electron capture process which populates a pair of single-particle orbitals, followed by 'spreading' of the two-electron states into chaotically mixed eigenstates. This method is similar to a configuration-average approach, as it neglects potentially important effects of spectator electrons and conservation of total angular momentum. In this work we develop a statistical theory which considers electron capture in...

  8. Effect of CuO on the efficiency of sulfur capture of Ca--based compounds during coal combustion

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    The efficiency of sulfur capture of CaO, Ca(OH)2 and CaCO3 as well as the effect of CuO on them were studied. Results showed that the efficiency of sulfur capture of Ca(OH)2 is the highest among these three compounds. When CuO was used with each of CaO, Ca(OH)2 and CaCO3 at the same time, the efficiency of all of them would rise, and that of Ca(OH)2 raise most. The efficiency of sulfur capture of Ca(OH)2 with CuO is 14.4% higher than that without CuO.

  9. Gallium metal affinity capture tandem mass spectrometry for the selective detection of phosphopeptides in complex mixtures

    OpenAIRE

    Blacken, Grady R.; Sadílek, Martin; Tureček, František

    2008-01-01

    Metal affinity capture tandem mass spectrometry (MAC-MSMS) is evaluated in a comparative study of a lysine-derived nitrilotriacetic acid (Nα, Nα-bis-(carboxymethyl)lysine, LysNTA) and an aspartic-acid-related iminodiacetic acid (N-(4-aminobutyl)aspartic acid, AspIDA) as selective phosphopeptide detection reagents. Both LysNTA and AspIDA spontaneously form ternary complexes with GaIII and phosphorylated amino acids and phosphopeptides upon mixing in solution. Collision-induced dissociation of ...

  10. Tag and Capture Flow Hydrogen Exchange Mass Spectrometry with a Fluorous-Immobilized Probe.

    Science.gov (United States)

    Marcsisin, Sean R; Liptak, Cary; Marineau, Jason; Bradner, James E; Engen, John R

    2015-06-16

    Analysis of complex mixtures of proteins by hydrogen exchange (HX) mass spectrometry (MS) is limited by one's ability to resolve the protein(s) of interest from the proteins that are not of interest. One strategy for overcoming this problem is to tag the target protein(s) to allow for rapid removal from the mixture for subsequent analysis. Here we illustrate a new solution involving fluorous conjugation of a retrievable probe. The appended fluorous tag allows for facile immobilization on a fluorous surface. When a target protein is passed over the immobilized probe molecule, it can be efficiently captured and then exposed to a flowing stream of deuterated buffer for hydrogen exchange. The utility of this method is illustrated for a model system of the Elongin BC protein complex bound to a peptide from HIV Vif. Efficient capture is demonstrated, and deuteration when immobilized was identical to deuteration in conventional solution-phase hydrogen exchange MS. Protein captured from a crude bacterial cell lysate could also be deuterated without the need for separate purification steps before HX MS. The advantages and disadvantages of the method are discussed in light of miniaturization and automation. PMID:26023704

  11. Detector development for a neutrino mass determination using the 163Ho electron capture spectrum

    International Nuclear Information System (INIS)

    The absolute scale of the neutrino mass eigenstates is one of the puzzles in modern particle physics and can be directly investigated using electroweak decays. In the context of the ECHO collaboration we are developing metallic magnetic calorimeters (MMCs) to be used with an internal 163Ho source to measure its electron capture (EC) spectrum. MMCs are calorimetric particle detectors with paramagnetic temperature sensor operated below 100 mK. The sensor converts the temperature rise of the detector, due to the absorption of an energetic particle, to a change of magnetization which is detected by a SQUID magnetometer. MMCs fulfill the requirements for cryogenic neutrino mass investigations, namely an energy resolution Δ EFWHM below 2 eV and pulse formation times of τ 163Ho obtained with our first detector prototype. We discuss the development of a 64 pixel array readout.

  12. Fluid flow and mass transfer characteristics of enhanced CO2 capture in a minichannel reactor

    International Nuclear Information System (INIS)

    Highlights: • Enhanced CO2 capture using aqueous DEA in a microreactor. • Observed flow patterns and calculated interfacial area by high-speed visualization. • Achieved close to 100% absorption efficiency under certain operating conditions. • Compared pressure drop and Sherwood number with predictions from model. • Mass transfer coefficient 2–4 orders of magnitude higher than conventional reactors. - Abstract: CO2 absorption using amine solvents can be significantly enhanced by the use of microscale reactors having high surface area to volume ratio. The present paper reports an experimental investigation of the fluid flow and mass transfer characteristics during reactive gas–liquid absorption in a minichannel reactor. Absorption of CO2 mixed with N2 into aqueous diethanolamine was studied in a channel having hydraulic diameter of 762 μm and a circular cross-sectional geometry. High-speed imaging of the two-phase flow was conducted to visualize the flow regimes. Image-processing analysis of the acquired flow patterns was performed to determine the interfacial area. The performance of the reactor was studied with respect to the absorption efficiency, pressure drop, mass transfer coefficient, interfacial area, enhancement factor, and Sherwood number. Parametric studies investigating the effects of phase superficial velocity, liquid reactant concentration, and CO2 concentration in the gas phase were performed and are discussed. High levels of absorption efficiency, close to 100%, were observed under certain operating conditions. An empirical model for the Sherwood number was developed and compared against experimental data. The mass transfer coefficient was found to be higher at reduced channel lengths, which was attributed to improved utilization of the absorption capacity of the amine solution for a given reactor volume. The presently achieved values of mass transfer coefficient and specific interfacial area are between 1 and 4 orders of magnitude

  13. Reaction 48Ca+208Pb: the capture-fission cross-sections and the mass-energy distributions of fragments above and deep below the Coulomb barrier

    OpenAIRE

    Prokhorova, E. V.; Cherepanov, E. A.; Itkis, M.G.; Kondratiev, N. A.; Kozulin, E. M.; Krupa, L.; Oganessian, Yu.Ts.; Pashkevich, V. V.; Pokrovsky, I. V.; Rusanov, A. Ya.

    2003-01-01

    The capture-fission cross-sections in an energy range of 206-242 MeV of 48Ca-projectiles and mass-energy distributions (MEDs) of reaction products in an energy range of 211-242 MeV have been measured in the 48Ca+208Pb reaction using the double-arm time-of-flight spectrometer CORSET. The MEDs of fragments for heated fission were shown to consist of two components. One component, which is due to classical fusion-fission, is associated with the symmetric fission of the 256No compound nucleus. Th...

  14. Evaluation and optimization of electron capture dissociation efficiency in fourier transform ion cyclotron resonance mass spectrometry.

    Science.gov (United States)

    McFarland, Melinda A; Chalmers, Michael J; Quinn, John P; Hendrickson, Christopher L; Marshall, Alan G

    2005-07-01

    Electron capture dissociation (ECD) efficiency has typically been lower than for other dissociation techniques. Here we characterize experimental factors that limit ECD and seek to improve its efficiency. Efficiency of precursor to product ion conversion was measured for a range of peptide (approximately 15% efficiency) and protein (approximately 33% efficiency) ions of differing sizes and charge states. Conversion of precursor ions to products depends on electron irradiation period and maximizes at approximately 5-30 ms. The optimal irradiation period scales inversely with charge state. We demonstrate that reflection of electrons through the ICR cell is more efficient and robust than a single pass, because electrons can cool to the optimal energy for capture, which allows for a wide range of initial electron energy. Further, efficient ECD with reflected electrons requires only a short (approximately 500 micros) irradiation period followed by an appropriate delay for cooling and interaction. Reflection of the electron beam results in electrons trapped in or near the ICR cell and thus requires a brief (approximately 50 micros) purge for successful mass spectral acquisition. Further electron irradiation of refractory precursor ions did not result in further dissociation. Possibly the ion cloud and electron beam are misaligned radially, or the electron beam diameter may be smaller than that of the ion cloud such that remaining precursor ions do not overlap with the electron beam. Several ion manipulation techniques and use of a large, movable dispenser cathode reduce the possibility that misalignment of the ion and electron beams limits ECD efficiency. PMID:15914017

  15. Advantages of external accumulation for electron capture dissociation in Fourier transform mass spectrometry.

    Science.gov (United States)

    Haselmann, K F; Budnik, B A; Olsen, J V; Nielsen, M L; Reis, C A; Clausen, H; Johnsen, A H; Zubarev, R A

    2001-07-01

    A combination of external accumulation (XA) with electron capture dissociation (ECD) improves the electron capture efficiency, shortens the analysis time, and allows for rapid integration of multiple scans in Fourier transform mass spectrometry. This improves the signal-to-noise ratio and increases the number of detected products, including structurally important MS3 fragments. With XA-ECD, the range of the labile species amenable to ECD is significantly extended. Examples include the first-time determination of the positions of six GalNAc groups in a 60-residue peptide, five sialic acid and six O-linked GalNAc groups in a 25-residue peptide, and the sulfate group position in a 11-residue peptide. Even weakly bound supramolecular aggregates, including nonspecific peptide complexes, can be analyzed with XA-ECD. Preliminary results are reported on high-rate XA-ECD that uses an indirectly heated dispenser cathode as an electron source. This shortens the irradiation time to > or = 1 ms and increases the acquisition rate to 3 scans/s, an improvement by a factor of 10-100. PMID:11467546

  16. The production of nitrogen-13 by neutron capture in boron compounds

    International Nuclear Information System (INIS)

    The 10B(α,n)13N reaction is studied as an activation process in a variety of solid boron-containing neutron shielding materials. The source of α-particles is the neutron capture reaction 10B(n,α)7Li. Samples of boron carbide, boron oxide, and boron nitride are irradiated with thermal neutrons and the rate of 13N production is determined. 13N promptly decays, emitting a positron. This positron efficiently annihilates with electrons in the material and the resultant 511 keV gamma ray is detected. For each of the above-mentioned materials, the rate of 13N production is (1-2) x 10-10 per captured neutron

  17. Rapid electron capture dissociation of mass-selectively accumulated oligodeoxynucleotide dications

    Science.gov (United States)

    Schultz, Kristin N.; Håkansson, Kristina

    2004-05-01

    We have performed extended characterization of the fragmentation patterns of oligodeoxynucleotide dications following electron capture dissociation (ECD) utilizing improved instrumentation. Our current results from a 9.4 T Fourier transform ion cyclotron resonance mass spectrometer equipped with mass-selective external ion accumulation and an indirectly heated dispenser cathode electron source demonstrate much richer fragmentation than from a previous 7 T instrument with a directly heated filament electron source. We propose the previous absence of backbone product ions from purine-containing oligonucleotides is a result of intramolecular hydrogen bonding, preventing product ions from separating. Similar behavior is observed at non-optimized ECD conditions with the current instrumentation. However, infrared laser heating of the resulting charge-reduced radical species results in extensive backbone fragmentation (different from infrared multiphoton dissociation) of the oligonucleotide dA6, demonstrating potential for ECD to characterize nucleic acid secondary structure. Under more optimized conditions, rich fragmentation, mostly in terms of w, (a/z-B), and (c/x-B) products, is observed for dA6, dC6, dG5, and d(GCATGC) following ECD only, allowing complete sequencing in several cases. The current ECD spectra contain some doubly charged products, indicating that populations of gas-phase oligodeoxynucleotide dications are zwitterionic.

  18. Detector development for a neutrino mass determination using the {sup 163}Ho electron capture spectrum

    Energy Technology Data Exchange (ETDEWEB)

    Ranitzsch, P.; Wegner, M.; Kempf, S.; Gamer, L.; Geist, J.; Hengstler, D.; Krantz, M.; Pavlov, E.; Pies, C.; Schaefer, S.; Uhl, S.; Wolf, T.; Fleischmann, A.; Enss, C.; Gastaldo, L. [Kirchhoff-Institute for Physics, Heidelberg University (Germany)

    2013-07-01

    The absolute scale of the neutrino mass eigenstates is one of the puzzles in modern particle physics and can be directly investigated using electroweak decays. In the context of the ECHO collaboration we are developing metallic magnetic calorimeters (MMCs) to be used with an internal {sup 163}Ho source to measure its electron capture (EC) spectrum. MMCs are calorimetric particle detectors with paramagnetic temperature sensor operated below 100 mK. The sensor converts the temperature rise of the detector, due to the absorption of an energetic particle, to a change of magnetization which is detected by a SQUID magnetometer. MMCs fulfill the requirements for cryogenic neutrino mass investigations, namely an energy resolution Δ E{sub FWHM} below 2 eV and pulse formation times of τ < 1 μs, as recently obtained with micro-fabricated MMCs for soft X-ray detection. We present the calorimetric measurement of the EC spectrum of {sup 163}Ho obtained with our first detector prototype. We discuss the development of a 64 pixel array readout.

  19. The development of new materials such MOFs for CO2 capture and alkylation of aromatic compounds

    International Nuclear Information System (INIS)

    This thesis is a European project TOPCOMBI of 22 partners. More specifically, this work is the result of collaboration between ENI (Italy), ITQ (Spain), Repsol (Spain) and IRCELYON (France). This work consists of 2 different themes which improvements can be obtained by finding new materials tailored to the needs. The global energy demands are and will be constantly rising in the coming years. In order to meet this need, new resources must be found and further optimized. Fossil fuels are among the most used resources in the world. Among this 3, natural gas appears to be the most promising point of view of energy efficiency and ecological impact. However, many gas fields cannot be treated because there are too small or too contaminated to be economically viable. One way to make them attractive is to lower the cost of purification using novel separation techniques such as the PSA system. However, there is no currently effective adsorbent to allow a viable economic cleansing. Today, the alkylation reactions represent a very important economic interest. Industrial processes are typically carried out by homogeneous acid reactions or not. Seeing the new environmental restrictions, some homogeneous catalytic processes must be replaced by heterogeneous catalytic reactions with the same yields. To do this, new materials to acid characters were used: the zeolites. However the small size of pores of these compounds prevents selective alkylation reactions of molecules too large compounds such as poly-aromatic. For twenty years, new microporous crystalline compounds have emerged: the MOFs, Metal Organic Frameworks. These compounds have the characteristic to be obtained with different metal cations and organic ligands. These combinations give a wide variety of these compounds at the level of reactivity, pore volume and pore size. In this work, we tried to get different materials with specific characteristics in order to use them in methods for purification of methane in acid

  20. -OH What? A Review of Mass Spectrometry Techniques for the Analysis of Phenolic Compounds

    OpenAIRE

    Kathyani Parasram

    2015-01-01

    Phenolic compounds, also called phenolics, are found in a variety of plant sources and can provide pharmacological and nutritive effects as well as taxonomic information. A single source can contain hundreds of phenolic compounds making characterization of these compounds time consuming and expensive. The recent leaps in mass spectrometry (MS) development including coupling to chromatographic columns, UV-vis, and tandem MS MS/MS) has renewed the study of phenolic compounds in both the agricul...

  1. Treatment of malignant melanoma by selective thermal neutron capture therapy using melanoma-seeking compound

    International Nuclear Information System (INIS)

    As pigment cells undergo melanoma genesis, accentuated melanogenesis concurrently occurs in principle. Subsequent to the understanding of intrinsic factors controlling both processes, we found our selective melanoma neutron capture therapy (NCT) using 10B-dopa (melanin substrate) analogue, 10B1-p-boronophenylalanine (10B1-BPA), followed by 10B(n, alpha)7Li reaction, induced by essentially harmless thermal neutrons, which releases energy of 2.33 MeV to 14 mu, the diameter of melanoma cells. In vitro/in vivo radiobiological analysis revealed the highly enhanced melanoma killing effect of 10B1-BPA. Chemical and prompt gamma ray spectrometry assays of 10B accumulated within melanoma cells after 10B1-BPA administration in vitro and in vivo show high affinity, e.g., 10B melanoma/blood ratio of 11.5. After successfully eradicating melanoma transplanted into hamsters with NCT, we advanced to preclinical studies using spontaneously occurring melanoma in Duroc pig skin. We cured three melanoma cases, 4.6 to 12 cm in diameter, by single neutron capture treatment. Complete disappearance of melanoma was obtained without substantial side effects. Acute and subacute toxicity as well as pharmacodynamics of 10B1-BPA have been studied in relation to therapeutic dosage requirements. Clinical radiation dosimetry using human phantom has been carried out. Further preclinical studies using human melanoma transplanted into nude mouse have been a useful model for obtaining optimal results for each melanoma type. We recently treated the first human melanoma patient with our NCT, using essentially the method for Duroc pig melanoma, and obtained similar regression time course leading to cure

  2. Desorption Mass Spectrometry for Nonvolatile Compounds Using an Ultrasonic Cutter

    Science.gov (United States)

    Habib, Ahsan; Ninomiya, Satoshi; Chen, Lee Chuin; Usmanov, Dilshadbek T.; Hiraoka, Kenzo

    2014-07-01

    In this work, desorption of nonvolatile analytes induced by friction was studied. The nonvolatile compounds deposited on the perfluoroalkoxy substrate were gently touched by an ultrasonic cutter oscillating with a frequency of 40 kHz. The desorbed molecules were ionized by a dielectric barrier discharge (DBD) ion source. Efficient desorption of samples such as drugs, pharmaceuticals, amino acids, and explosives was observed. The limits of detection for these compounds were about 1 ng. Many compounds were detected in their protonated forms without undergoing significant fragmentation. When the DBD was off, no ions for the neutral samples could be detected, meaning that only desorption along with little ionization took place by the present technique.

  3. Surface water mass composition changes captured by cores of Arctic land-fast sea ice

    Science.gov (United States)

    Smith, I. J.; Eicken, H.; Mahoney, A. R.; Van Hale, R.; Gough, A. J.; Fukamachi, Y.; Jones, J.

    2016-04-01

    In the Arctic, land-fast sea ice growth can be influenced by fresher water from rivers and residual summer melt. This paper examines a method to reconstruct changes in water masses using oxygen isotope measurements of sea ice cores. To determine changes in sea water isotope composition over the course of the ice growth period, the output of a sea ice thermodynamic model (driven with reanalysis data, observations of snow depth, and freeze-up dates) is used along with sea ice oxygen isotope measurements and an isotopic fractionation model. Direct measurements of sea ice growth rates are used to validate the output of the sea ice growth model. It is shown that for sea ice formed during the 2011/2012 ice growth season at Barrow, Alaska, large changes in isotopic composition of the ocean waters were captured by the sea ice isotopic composition. Salinity anomalies in the ocean were also tracked by moored instruments. These data indicate episodic advection of meteoric water, having both lower salinity and lower oxygen isotopic composition, during the winter sea ice growth season. Such advection of meteoric water during winter is surprising, as no surface meltwater and no local river discharge should be occurring at this time of year in that area. How accurately changes in water masses as indicated by oxygen isotope composition can be reconstructed using oxygen isotope analysis of sea ice cores is addressed, along with methods/strategies that could be used to further optimize the results. The method described will be useful for winter detection of meteoric water presence in Arctic fast ice regions, which is important for climate studies in a rapidly changing Arctic. Land-fast sea ice effective fractionation coefficients were derived, with a range of +1.82‰ to +2.52‰. Those derived effective fractionation coefficients will be useful for future water mass component proportion calculations. In particular, the equations given can be used to inform choices made when

  4. Comprehensive two-dimensional gas chromatography - time-of-flight mass spectrometry and simultaneous electron capture detection/nitrogen phosphorous detection for incense analysis

    Science.gov (United States)

    Tran, Tin C.; Marriott, Philip J.

    This study reports comprehensive two-dimensional gas chromatography hyphenated to time-of-flight mass spectrometry detection (GC × GC/TOFMS) for characterisation and identification of components generated by four different types of powdered incense headspace (H/S) and incense smoke. GC × GC/TOFMS allowed simultaneous separation and identification of compounds emitted into the atmosphere as a result of combustion of incense powder. The smoke stream comprised compounds originating from the incense powder, and combustion products such as saturated and unsaturated hydrocarbons, essential oil type compounds, nitromusks, fatty acid methyl esters (FAMEs), polycyclic aromatic hydrocarbons (PAHs, which possibly include oxygenated and nitrated PAH), N-heterocyclics, pyrans and furans, which were detected and tentatively identified by GC × GC/TOFMS. GC × GC-electron capture detector/nitrogen phosphorous detector (ECD/NPD) potentially offers the prospect of providing selective chemical compositional information of incense powder and smoke, such as nitrogen-containing (N-containing) and halogenated compounds. Results of GC×GC-ECD/NPD showed that both incense powder and smoke generated emission of N-containing and halogenated compounds. A significant number of halogenated and N-containing compounds were emitted during the incomplete combustion of incense. However, one further objective of this paper is to demonstrate the capacity of comprehensive two-dimensional gas chromatography coupled to specific and/or selective detectors such as those used in this study (GC × GC-ECD/NPD) for the detection of particular classes of compounds such as N-containing and halogenated compounds at trace level concentrations in complex smoke samples.

  5. D Capturing Performances of Low-Cost Range Sensors for Mass-Market Applications

    Science.gov (United States)

    Guidi, G.; Gonizzi, S.; Micoli, L.

    2016-06-01

    Since the advent of the first Kinect as motion controller device for the Microsoft XBOX platform (November 2010), several similar active and low-cost range sensing devices have been introduced on the mass-market for several purposes, including gesture based interfaces, 3D multimedia interaction, robot navigation, finger tracking, 3D body scanning for garment design and proximity sensors for automotive. However, given their capability to generate a real time stream of range images, these has been used in some projects also as general purpose range devices, with performances that for some applications might be satisfying. This paper shows the working principle of the various devices, analyzing them in terms of systematic errors and random errors for exploring the applicability of them in standard 3D capturing problems. Five actual devices have been tested featuring three different technologies: i) Kinect V1 by Microsoft, Structure Sensor by Occipital, and Xtion PRO by ASUS, all based on different implementations of the Primesense sensor; ii) F200 by Intel/Creative, implementing the Realsense pattern projection technology; Kinect V2 by Microsoft, equipped with the Canesta TOF Camera. A critical analysis of the results tries first of all to compare them, and secondarily to focus the range of applications for which such devices could actually work as a viable solution.

  6. -OH What? A Review of Mass Spectrometry Techniques for the Analysis of Phenolic Compounds

    Directory of Open Access Journals (Sweden)

    Kathyani Parasram

    2015-12-01

    Full Text Available Phenolic compounds, also called phenolics, are found in a variety of plant sources and can provide pharmacological and nutritive effects as well as taxonomic information. A single source can contain hundreds of phenolic compounds making characterization of these compounds time consuming and expensive. The recent leaps in mass spectrometry (MS development including coupling to chromatographic columns, UV-vis, and tandem MS MS/MS has renewed the study of phenolic compounds in both the agricultural and medical fields through its capability for fast, accurate and high throughput analyses. This paper will summarize recent discoveries, methodologies, and applications of MS in studies of phenolic compounds.

  7. COMPARISON OF SIMCA PATTERN RECOGNITION & LIBRARY SEARCH IDENTIFICATION OF HAZARDOUS COMPOUNDS FROM MASS SPECTRA

    Science.gov (United States)

    SIMCA pattern recognition methods have been applied to mass spectral data from a target list of hazardous chemicals. cheme has been proposed for classification and identification of five classes of compounds including aromatics, chlorocarbons, bromocarbons, hydrocarbons, and poly...

  8. COMPARISON OF SIMCA PATTERN RECOGNITION AND LIBRARY SEARCH IDENTIFICATION OF HAZARDOUS COMPOUNDS FROM MASS SPECTRA

    Science.gov (United States)

    SIMCA pattern recognition methods have been applied to mass spectral data from a target list of hazardous chemicals. cheme has been proposed for classification and identification of five classes of compounds including aromatics, chlorocarbons, bromocarbons, hydrocarbons, and poly...

  9. Nanogram-Scale Preparation and NMR Analysis for Mass-Limited Small Volatile Compounds

    OpenAIRE

    Nojima, Satoshi; Kiemle, David J.; Francis X Webster; Apperson, Charles S.; Schal, Coby

    2011-01-01

    Semiochemicals are often produced in infinitesimally small quantities, so their isolation requires large amounts of starting material, not only requiring significant effort in sample preparation, but also resulting in a complex mixture of compounds from which the bioactive compound needs to be purified and identified. Often, compounds cannot be unambiguously identified by their mass spectra alone, and NMR analysis is required for absolute chemical identification, further exacerbating the situ...

  10. Preparation of a radioactive boron compound (B-I-131-lipiodol) for neutron capture therapy of hepatoma

    International Nuclear Information System (INIS)

    In our research, a radioactive boron compound, B-I-131-lipiodol, that can be selectively retained in hepatoma cells was prepared. Combining the effect of α particles produced by boron neutron capture reaction with the β particles released by radionuclides in the radioactive boron compounds will produce a synergistic killing effect on cancer cells. Human hepatoma HepG2 cell cultures were used to examine the stability and the intracellular distribution of the radioactive boron drug. Microscopes were used to examine the interaction and retention of B-I-131-lipiodol globules in the individual hepatoma cell. Moreover, ICP-AES and NaI scintillation counter were performed to determine boron concentrations and I-131 radioactivity, respectively. Results showed that B-I-131-lipiodol with a boron concentration and a specific radioactivity ranged from 500-2000 ppm and 0.05-10 mCi/mL respectively was stably retained in serum. The radiochemical purity of B-I-131-lipiodol was 98%. After supplement with a medium containing B-I-131-lipiodol, the HepG2 cells had intracellular B-I-131-lipiodol globules in the cytoplasm as seen by inverted light microscope, the I-131 and boron can be stably retained in HepG2 cells. (author)

  11. Application of the boron neutron capture therapy to undifferentiated thyroid cancer using two boron compounds (BPA and BOPP)

    International Nuclear Information System (INIS)

    We have shown the selective uptake of boronophenylalanine (BPA) by undifferentiated thyroid cancer (UTC) human cell line ARO, both in vitro and in vivo. Moreover, a 50% histologic cure of mice bearing the tumor was observed when the complete boron neutron capture therapy was applied. More recently we have analyzed the biodistribution of BOPP (tetrakis-carborane carboxylate ester of 2,4-bis-(ba-dihydroxyethyl)-deutero-porphyrin IX) and showed that when BOPP was injected 5 days before BPA, and the animals were sacrificed 60 min after the ip injection of BPA, a significant increase in boron uptake by the tumor was found (38-45ppm with both compounds Vs. 20 ppm with BPA alone). Five days post the ip BOPP injection and 1 hr after BPA, the ratios were: tumor/blood 3,75; tumor /distal skin 2. Other important ratios were tumor/thyroid 6,65 and tumor/lung 3,8. The present studies were performed in mice transplanted with ARO cells and injected with BOPP and BPA. Only in mice treated with the neutron beam and injected with the boronated compounds we observed a 100% control of tumor growth. Two groups of mice received different total absorbed doses: 3.00 and 6.01 Gy, but no further improvement in the outcome was found compared to the previous results using BPA alone (4.3 Gy). (author)

  12. Study of electrospray ionization tandem mass spectrometry of the benzofuranone compounds

    Institute of Scientific and Technical Information of China (English)

    Zhan Qi Niu; Yu Min Sun; Feng Niu; Jian Han; Da Wei Chen

    2008-01-01

    A detailed analysis of benzofuranone compounds under multiple tandem mass spectrometry (ESI-MS(n)) conditions is reported. Element composition data of the fragment ions were obtained with the aid of comparison of the multiple tandem mass spectra of four compounds, and the structures of which are identical except for some substituted groups or epimers or ra-r/ww-isomers. Attempts have been made to provide rational pathways for the formation of the fragment ions from these protonated compounds. And the structure-fragmentation relationships will facilitate the characterization of the structures of other analogs.

  13. Biodistribution of Boron compounds in an experimental model of liver metastases for Boron Neutron Capture (BNCT) Studies

    International Nuclear Information System (INIS)

    Boron Neutron Capture Therapy (BNCT) is a binary treatment modality that involves the selective accumulation of 10B carriers in tumors followed by irradiation with thermal or epithermal neutrons. The high linear energy transfer alpha particles and recoiling 7Li nuclei emitted during the capture of a thermal neutron by a 10B nucleus have a short range and a high biological effectiveness. Thus, BNCT would potentially target neoplastic tissue selectively. In previous studies we demonstrated the therapeutic efficacy of different BNCT protocols in an experimental model of oral cancer. More recently we performed experimental studies in normal rat liver that evidenced the feasibility of treating liver metastases employing a novel BNCT protocol proposed by JEC based on ex-situ treatment and partial liver auto-transplant. The aim of the present study was to perform biodistribution studies with different boron compounds and different administration protocols to determine the protocols that would be therapeutically useful in 'in vivo' BNCT studies at the RA-3 Nuclear Reactor in an experimental model of liver metastases in rats. Materials and Methods. A total of 70 BDIX rats (Charles River Lab., MA, USA) were inoculated in the liver with syngeneic colon cancer cells DH/DK12/TRb (ECACC, UK) to induce the development of subcapsular metastatic nodules. 15 days post-inoculation the animals were used for biodistribution studies. A total of 11 protocols were evaluated employing the boron compounds boronophenylalanine (BPA) and GB-10 (Na210B1-0H10), alone or combined employing different doses and administration routes. Tumor, normal tissue and blood samples were processed for boron measurement by ICP-OES. Results. Several protocols proved potentially useful for BNCT studies in terms of absolute boron concentration in tumor and preferential uptake of boron by tumor tissue, i.e. BPA 15.5 mg 10B/kg iv + GB-10 50 mg 10B/kg iv; BPA 46.5 mg 10B/kg ip; BPA 46.5 mg 10B/kg ip + iv; BPA 46

  14. Probing the Electron Capture Dissociation Mass Spectrometry of Phosphopeptides with Traveling Wave Ion Mobility Spectrometry and Molecular Dynamics Simulations

    OpenAIRE

    Kim, Doyong; Pai, Pei-Jing; Creese, Andrew J.; Jones, Andrew W.; Russell, David H.; Cooper, Helen J.

    2015-01-01

    Electron capture dissociation mass spectrometry offers several advantages for the analysis of peptides, most notably that backbone c and z fragments typically retain labile modifications such as phosphorylation. We have shown previously that, in some cases, the presence of phosphorylation has a deleterious effect on peptide sequence coverage, and hypothesized that intramolecular interactions involving the phosphate group were preventing separation of backbone fragments. In the present work, w...

  15. A measurement of actinide neutron transmutations with accelerator mass spectrometry in order to infer neutron capture cross sections

    Science.gov (United States)

    Bauder, William K.

    Improved neutron capture cross section data for transuranic and minor actinides are essential for assessing possibilities for next generation reactors and advanced fuel cycles. The Measurement of Actinide Neutron TRAnsmutation (MANTRA) project aims to make a comprehensive set of energy integrated neutron capture cross section measurements for all relevant isotopes from Th to Cf. The ability to extract these cross sections relies on the use of Accelerator Mass Spectrometry (AMS) to analyze isotopic concentrations in samples irradiated in the Advanced Test Reactor (ATR). The AMS measurements were performed at the Argonne Tandem Linear Accelerator System (ATLAS) and required a number of key technical developments to the ion source, accelerator, and detector setup. In particular, a laser ablation material injection system was developed at the electron cyclotron resonance ion source. This system provides a more effective method to produce ion beams from samples containing only 1% actinide material and offers some benefits for reducing cross talk in the source. A series of four actinide measurements are described in this dissertation. These measurements represent the most substantial AMS work attempted at ATLAS and the first results of the MANTRA project. Isotopic ratios for one and two neutron captures were measured in each sample with total uncertainties around 10%. These results can be combined with a MCNP model for the neutron fluence to infer actinide neutron capture cross sections.

  16. Large scale localization of protein phosphorylation by use of electron capture dissociation mass spectrometry.

    OpenAIRE

    Sweet, Steve M.M.; Bailey, Christopher M; Cunningham, Debbie L.; Heath, John K.; Cooper, Helen J.

    2009-01-01

    We used on-line electron capture dissociation (ECD) for the large scale identification and localization of sites of phosphorylation. Each FT-ICR ECD event was paired with a linear ion trap collision-induced dissociation (CID) event, allowing a direct comparison of the relative merits of ECD and CID for phosphopeptide identification and site localization. Linear ion trap CID was shown to be most efficient for phosphopeptide identification, whereas FT-ICR ECD was superior for localization of si...

  17. Large Scale Localization of Protein Phosphorylation by Use of Electron Capture Dissociation Mass Spectrometry * S⃞

    OpenAIRE

    Sweet, Steve M.M.; Bailey, Christopher M; Cunningham, Debbie L.; Heath, John K.; Cooper, Helen J.

    2009-01-01

    We used on-line electron capture dissociation (ECD) for the large scale identification and localization of sites of phosphorylation. Each FT-ICR ECD event was paired with a linear ion trap collision-induced dissociation (CID) event, allowing a direct comparison of the relative merits of ECD and CID for phosphopeptide identification and site localization. Linear ion trap CID was shown to be most efficient for phosphopeptide identification, whereas FT-ICR ECD was superior for localization of si...

  18. A Thermal Desorption Chemical Ionization Mass Spectrometer for the In Situ Measurement of Aerosol Organic Compounds

    Science.gov (United States)

    Thornberry, T.; Murphy, D. M.; Lovejoy, E. R.

    2005-12-01

    Organic material has been observed to comprise a significant fraction of organic aerosol mass in many regions of the troposphere. The organic compounds that comprise the organic fraction of atmospheric aerosol have the potential to affect the radiative and microphysical properties of the aerosol, with concomitant impacts on the role of the aerosol in climate forcing through direct and indirect effects. Knowledge of the organic compounds in atmospheric aerosols and their spatial distribution is needed to determine their effect on aerosol properties as well as to elucidate the role of aerosols in the chemistry of the atmosphere. The speciated measurement of aerosol organic compounds poses a significant experimental challenge due to the complexity and large number of organic species, and the low concentration at which individual species are present. A prototype instrument has been designed and built to make in situ speciated measurements of aerosol organic compounds. The instrument is composed of an aerosol collection/thermal desorption inlet coupled to a custom chemical ionization ion trap mass spectrometer. Aerosols are collected over a variable time by impaction on a target stage. The stage is then rapidly heated to volatilize the organic compounds into a small flow of helium carrier gas and conveyed to an ion-molecule reaction drift tube where proton transfer from H3O+ is used to softly ionize organic species. The ionized analyte molecules are then trapped and mass analyzed using a quadrupole ion trap. Results from preliminary experiments using laboratory-generated aerosol will be discussed

  19. Detection of trace levels of triclopyr using capillary gas chromatography-electron-capture negative-ion chemical ionization mass spectrometry.

    Science.gov (United States)

    Begley, P; Foulger, B E

    1988-04-01

    Triclopyr, after esterification, is shown to be a suitable candidate for detection by gas chromatography-electron-capture negative-ion chemical ionization mass spectrometry forming a characteristic carboxylate anion which offers a high detection sensitivity. A detection limit of 70 fg reaching the ionizer is indicated. Low backgrounds and an absence of chemical interferences are shown for vegetation extracts, using a simple method of extraction and derivatisation. A similar behaviour is demonstrated for 2,4-D and 2,4,5-T. PMID:3379116

  20. PATTERN RECOGNITION/EXPERT SYSTEM FOR IDENTIFICATION OF TOXIC COMPOUNDS FROM LOW RESOLUTION MASS SPECTRA

    Science.gov (United States)

    An empirical rule-based pattern recognition/expert system for classifying, estimating molecular weights and identifying low resolution mass spectra of toxic and other organic compounds has been developed and evaluated. he system was designed to accommodate low concentration spect...

  1. Compound classification by computer treatment of low resolution mass spectra - Application to geochemical and environmental problems.

    Science.gov (United States)

    Smith, D. H.; Eglinton, G.

    1972-01-01

    A description is given of a development of computer analysis of low-resolution chromatographic-mass spectrometric data, which provides a preliminary classification of an unknown spectrum as a listing of candidate classes of compounds. This procedure, referred to as COMSOC (Classification of Mass Spectra on Computers), operates by converting an incoming unknown mass spectrum into a simplified key word which is then compared with each of the key words held in its reference file. The advantages of COMSOC in characterizing complex mixtures are emphasized.

  2. Computational Prediction of Electron Ionization Mass Spectra to Assist in GC/MS Compound Identification.

    Science.gov (United States)

    Allen, Felicity; Pon, Allison; Greiner, Russ; Wishart, David

    2016-08-01

    We describe a tool, competitive fragmentation modeling for electron ionization (CFM-EI) that, given a chemical structure (e.g., in SMILES or InChI format), computationally predicts an electron ionization mass spectrum (EI-MS) (i.e., the type of mass spectrum commonly generated by gas chromatography mass spectrometry). The predicted spectra produced by this tool can be used for putative compound identification, complementing measured spectra in reference databases by expanding the range of compounds able to be considered when availability of measured spectra is limited. The tool extends CFM-ESI, a recently developed method for computational prediction of electrospray tandem mass spectra (ESI-MS/MS), but unlike CFM-ESI, CFM-EI can handle odd-electron ions and isotopes and incorporates an artificial neural network. Tests on EI-MS data from the NIST database demonstrate that CFM-EI is able to model fragmentation likelihoods in low-resolution EI-MS data, producing predicted spectra whose dot product scores are significantly better than full enumeration "bar-code" spectra. CFM-EI also outperformed previously reported results for MetFrag, MOLGEN-MS, and Mass Frontier on one compound identification task. It also outperformed MetFrag in a range of other compound identification tasks involving a much larger data set, containing both derivatized and nonderivatized compounds. While replicate EI-MS measurements of chemical standards are still a more accurate point of comparison, CFM-EI's predictions provide a much-needed alternative when no reference standard is available for measurement. CFM-EI is available at https://sourceforge.net/projects/cfm-id/ for download and http://cfmid.wishartlab.com as a web service. PMID:27381172

  3. Accelerator mass spectrometry analysis of aroma compound absorption in plastic packaging materials

    Science.gov (United States)

    Stenström, Kristina; Erlandsson, Bengt; Hellborg, Ragnar; Wiebert, Anders; Skog, Göran; Nielsen, Tim

    1994-05-01

    Absorption of aroma compounds in plastic packaging materials may affect the taste of the packaged food and it may also change the quality of the packaging material. A method to determine the aroma compound absorption in polymers by accelerator mass spectrometry (AMS) is being developed at the Lund Pelletron AMS facility. The high sensitivity of the AMS method makes it possible to study these phenomena under realistic conditions. As a first test low density polyethylene exposed to 14C-doped ethyl acetate is examined. After converting the polymer samples with the absorbed aroma compounds to graphite, the {14C }/{13C } ratio of the samples is measured by the AMS system and the degree of aroma compound absorption is established. The results are compared with those obtained by supercritical fluid extraction coupled to gas chromatography (SFE-GC).

  4. Probing the Electron Capture Dissociation Mass Spectrometry of Phosphopeptides with Traveling Wave Ion Mobility Spectrometry and Molecular Dynamics Simulations

    Science.gov (United States)

    Kim, Doyong; Pai, Pei-Jing; Creese, Andrew J.; Jones, Andrew W.; Russell, David H.; Cooper, Helen J.

    2015-06-01

    Electron capture dissociation mass spectrometry offers several advantages for the analysis of peptides, most notably that backbone c and z fragments typically retain labile modifications such as phosphorylation. We have shown previously that, in some cases, the presence of phosphorylation has a deleterious effect on peptide sequence coverage, and hypothesized that intramolecular interactions involving the phosphate group were preventing separation of backbone fragments. In the present work, we seek to rationalize the observed ECD behavior through a combination of ECD of model peptides, traveling wave ion mobility mass spectrometry and molecular dynamics simulations. The results suggest that for doubly protonated ions of phosphopeptide APLpSFRGSLPKSYVK a salt-bridge structure is favored, whereas for the doubly-protonated ions of APLSFRGSLPKpSYVK ionic hydrogen bonds predominate.

  5. Target Capturing Control for Space Robots with Unknown Mass Properties: A Self-Tuning Method Based on Gyros and Cameras.

    Science.gov (United States)

    Li, Zhenyu; Wang, Bin; Liu, Hong

    2016-01-01

    Satellite capturing with free-floating space robots is still a challenging task due to the non-fixed base and unknown mass property issues. In this paper gyro and eye-in-hand camera data are adopted as an alternative choice for solving this problem. For this improved system, a new modeling approach that reduces the complexity of system control and identification is proposed. With the newly developed model, the space robot is equivalent to a ground-fixed manipulator system. Accordingly, a self-tuning control scheme is applied to handle such a control problem including unknown parameters. To determine the controller parameters, an estimator is designed based on the least-squares technique for identifying the unknown mass properties in real time. The proposed method is tested with a credible 3-dimensional ground verification experimental system, and the experimental results confirm the effectiveness of the proposed control scheme. PMID:27589748

  6. Identification of tartary buckwheat tea aroma compounds with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Qin, Peiyou; Ma, Tingjun; Wu, Li; Shan, Fang; Ren, Guixing

    2011-08-01

    Tartary buckwheat tea, which is an important and healthy product, has a distinct malty aroma. However, its characteristic aroma compounds have not been elucidated. The aims of present study were identification and quantification of its aroma compounds. The analyses were performed by gas chromatography-mass spectrometry (GC-MS) after 3 different isolation techniques. Seventy-seven compounds were identified. Among these compounds, 35 were quantified by available standards. The compounds with a high probability of contribution to the tartary buckwheat tea aroma (OAV ≥ 10) were as follows: 2,5-dimethyl-4-hydroxy-3(2H)-furanone, nonanal, 2,3-diethyl-5-methylpyrazine, benzeneacetaldehyde, maltol, 2,5-dimethylpyrazine, 2-ethyl-5-methylpyrazine, trimethylpyrazine. Some nutritional and bioactive compounds were also identified in this study, such as linoleic acid, niacin, vanillic acid, 7-hydroxycoumarin, butylated hydroxytoluene. Practical Application: Tartary buckwheat, one type of buckwheat, has gained much attention from nutritionists and medical doctors in recent years. It is rich in rutin, quercetin, and other nutrients that are good for health. Tartary buckwheat-based product such as tartary buckwheat tea is an important and popular healthy product in China, Japan,South Korea, European countries as well as in American countries. It has a distinct malty aroma. The present study first identified and quantified of its aroma compounds. The results will draw attention to other researchers in food flavor and buckwheat filed. PMID:22417522

  7. Analysis of volatile compounds of Malaysian Tualang (Koompassia excelsa) honey using gas chromatography mass spectrometry.

    Science.gov (United States)

    Nurul Syazana, M S; Gan, S H; Halim, A S; Shah, Nurul Syazana Mohamad; Gan, Siew Hua; Sukari, Halim Ahmad

    2013-01-01

    The constituents of honey's volatile compounds depend on the nectar source and differ depending on the place of origin. To date, the volatile constituents of Tualang honey have never been investigated. The objective of this study was to analyze the volatile compounds in local Malaysian Tualang honey. A continuous extraction of Tualang honey using five organic solvents was carried out starting from non-polar to polar solvents and the extracted samples were analysed using gas chromatography-mass spectrometry (GC-MS). Overall, 35 volatile compounds were detected. Hydrocarbons constitute 58.5% of the composition of Tualang honey. Other classes of chemical compounds detected included acids, aldehydes, alcohols, ketones, terpenes, furans and a miscellaneous group. Methanol yielded the highest number of extracted compounds such as acids and 5-(Hydroxymethyl) furfural (HMF). This is the first study to describe the volatile compounds in Tualang honey. The use of a simple one tube, stepwise, non-thermal liquid-liquid extraction of honey is a advantageous as it prevents sample loss. Further research to test the clinical benefits of these volatile compounds is recommended. PMID:24146441

  8. A new technique for the determination of impurities in uranium-and thorium compounds, by the analysis of capture gamma rays

    International Nuclear Information System (INIS)

    A new technique is presented for the determination of impurities in uranium-and thorium compounds, based on the analysis of capture gamma rays emitted by the impurities and by the matrix element, without previous matrix isolation. The experimental system utilized is described and calibration curves are given. Several measurements are made for uranium oxide and thorium oxide samples to which known impurities were added in a controlled way: Through the analysis of spectra, the possibility is shown of utilizing the new technique for the determination of impurities found in uranium-and thorium compounds used as nuclear fuel materials. (Author)

  9. Recent measurements of neutron capture cross sections in the fission product mass region

    International Nuclear Information System (INIS)

    The radiative capture cross sections for the separated isotopes of Sr, Y, Zr, Mo, Pd, Cd, Ba, La, Ce, Pr and Nd in the energy range 3 to 200 keV were measured with high energy resolution at the 40 m station of the Oak Ridge Electron Linear Accelerator. Maxwellian averaged 30 keV cross sections and average resonance parameters derived from the analysis are tabulated. A strong dependence of the average radiative widths on neutron binding energy is noted. This leads to a pronounced even-odd disparity. Neutron strength functions reduce with decreasing binding energy along an isotopic chain owing to the decreasing density of doorway states at the binding energy. 16 references

  10. Optimization of MALDI-TOF MS Detection for Enhanced Sensitivity of Affinity-Captured Proteins Spanning a 100 kDa Mass Range

    OpenAIRE

    Gatlin-Bunai, Christine L.; Lisa H. Cazares; Cooke, William E.; Semmes, Oliver J.; Malyarenko, Dariya I.

    2007-01-01

    Analysis of complex biological samples by MALDI-TOF mass spectrometry has been generally limited to the detection of low-mass protein (or protein fragment) peaks. We have extended the mass range of MALDI-TOF high-sensitivity detection by an order of magnitude through the combined optimization of instrument parameters, data processing, and sample preparation procedures for affinity capture. WCX, C3, and IMAC magnetic beads were determined to be complementary and most favorable for broad mass r...

  11. Improved method for estimating molecular weights of volatile organic compounds from low-resolution mass spectra

    Energy Technology Data Exchange (ETDEWEB)

    Scott, D.R.

    1991-01-01

    An improved method of estimating molecular weights of volatile organic compounds from their mass spectra has been developed and implemented with an expert system. The method is based on the strong correlation of MAXMASS, the highest mass with an intensity of 5% of the base peak in a mass spectrum, with the true molecular weight. Linear corrections to MAXMASS, which yield molecular weight estimates, were derived empirically using the expert system. The system is based on a sequential modular design with a primary classifier linked to molecular weight estimators for the resulting six classes. These are non-halobenzenes; chlorobenzenes; bromoalkenes/alkenes; mono- and dichloroalkanes/alkenes; tri-, tetra- and pentachloro-alkanes/alkenes; and others. Performance tests were made with the old and improved expert systems and the Self Training Interpretive and Retrieval System (STIRS) on NIST reference spectra of the 107 training compounds; on a set of 32 test NIST reference spectra of other compounds found in air samples; on a set of 100 randomly selected NIST reference spectra; and on 27 spectra taken from actual field gas chromatography/mass spectrometry samples.

  12. Evolution of 8-10 solar mass stars toward electron capture supernovae. II - Collapse of an O + NE + MG core

    Science.gov (United States)

    Nomoto, Ken'ichi

    1987-11-01

    In this paper, the helium core of an 8.8 solar mass star is evolved from the helium-burning stage through the early stage of collapse of an O + Ne + Mg core. The star undergoes helium and carbon burning under nondegenerate conditions and leaves an O + Ne + Mg core. The penetration of the surface convection zone into the helium layer starts much earlier than in a 9.6 solar mass star studied elsewhere. The subsequent evolution is brought about by hydrogen-helium double-shell burning. The mass interior to the helium-burning shell, M(Heb), increases toward the Chandrasekhar limit. After M(Heb) reaches 1.375 solar mass, electron captures on Mg-24, Na-24, Ne-20, and F-20 take place. The electron concentration decreases, the resulting rapid core contraction ignites the oxygen deflagration, and the material undergoes incineration into nuclear statistical equilibrium at the oxygen deflagration front. The collapse of the core is accelerated, and the oxygen deflagration front advances.

  13. NMR and mass spectrometry in structural characterization of new organometallic compounds

    International Nuclear Information System (INIS)

    Nuclear magnetic resonance (NMR) and mass spectrometry (MS) are very useful tools in the investigation of both organometallic and coordination compounds giving information about their molecular structure and their chemical reactivity. New derivatives, either of main group (14-16) or transition metals (tungsten) were prepared. They were structurally characterized using 1D (multinuclear) and 2D NMR spectroscopy and various mass spectrometry methods (EI, CI, FAB, MALDI-TOF). Complementary structural information for some ansa-metallocenes of tungsten as well as for several organometallic derivatives and complexes of the group 14-16 metals are discussed. (author)

  14. Compound coverage enhancement of electrospray ionization mass spectrometry through the addition of a homemade needle.

    Science.gov (United States)

    Xiao, Shun; Qian, Shuai; Wang, Yi; Zhang, Yufeng; Cheng, Yiyu

    2013-03-21

    The response of many previously low-detectable or undetectable compounds in electrospray ionization mass spectrometry (ESI-MS) has been enhanced by the addition of a simple, homemade needle into the traditional ESI interface. The needle located between the ESI emitter and the ion sweep cone (inlet of the detector) would ionize those neutral gaseous compounds, formed during electrospray, by a corona discharge process. The mobile phases, ESI parameters and positions of the needle were investigated and optimized. Several groups of compounds and herbal extracts were tested using the homemade set-up. Both the results of the flow injection and the hyphenated MS analyses showed significant enhancement effects of our homemade needle. The advantages of the proposed method include low cost, simplicity and practicality. PMID:23364279

  15. Effective atomic numbers and mass attenuation coefficients of some thermoluminescent dosimetric compounds for total photon interaction

    International Nuclear Information System (INIS)

    Effective atomic numbers for total gamma-ray interaction with some selected thermoluminescent dosimetric compounds such as barium acetate, barium sulfate, calcium carbonate, calcium sulfate, calcium sulfate dihydrate, cadmium sulfate (anhydrous), cadmium sulfate, strontium sulfate, and lithium fluoride have been calculated in the 1-keV to 20-MeV energy region. Experimental mass attenuation coefficients and effective atomic numbers for these compounds at selected photon energies of 26.3, 33.2, 59.54, and 661.6 keV have been obtained from good geometry transmission measurements and compared with theoretical values. The effect of absorption edge on effective atomic numbers and its variation with energy, and nonvalidity of the Bragg's mixture rule at incident photon energies closer to the absorption edges of constituent elements of compounds are discussed

  16. Real-time monitoring of volatile organic compounds using chemical ionization mass spectrometry

    Science.gov (United States)

    Mowry, Curtis Dale; Thornberg, Steven Michael

    1999-01-01

    A system for on-line quantitative monitoring of volatile organic compounds (VOCs) includes pressure reduction means for carrying a gaseous sample from a first location to a measuring input location maintained at a low pressure, the system utilizing active feedback to keep both the vapor flow and pressure to a chemical ionization mode mass spectrometer constant. A multiple input manifold for VOC and gas distribution permits a combination of calibration gases or samples to be applied to the spectrometer.

  17. Measuring Nitrous Oxide Mass Transfer into Non-Aqueous CO2BOL CO2 Capture Solvents

    Energy Technology Data Exchange (ETDEWEB)

    Whyatt, Greg A.; Freeman, Charles J.; Zwoster, Andy; Heldebrant, David J.

    2016-03-28

    This paper investigates CO2 absorption behavior in CO2BOL solvents by decoupling the physical and chemical effects using N2O as a non-reactive mimic. Absorption measurements were performed using a wetted-wall contactor. Testing was performed using a “first generation” CO2 binding organic liquid (CO2BOL), comprised of an independent base and alcohol. Measurements were made with N2O at a lean (0.06 mol CO2/mol BOL) and rich (0.26 mol CO2/mol BOL) loading, each at three temperatures (35, 45 and 55 °C). Liquid-film mass transfer coefficients (kg') were calculated by subtracting the gas film resistance – determined from a correlation from literature – from the overall mass transfer measurement. The resulting kg' values for N2O in CO2BOLs were found to be higher than that of 5 M aqueous MEA under comparable conditions, which is supported by published measurements of Henry’s coefficients for N2O in various solvents. These results suggest that the physical solubility contribution for CO2 absorption in CO2BOLs is greater than that of aqueous amines, an effect that may pertain to other non-aqueous solvents.

  18. AN INTEGRAL REACTOR PHYSICS EXPERIMENT TO INFER ACTINIDE CAPTURE CROSS-SECTIONS FROM THORIUM TO CALIFORNIUM WITH ACCELERATOR MASS SPECTROMETRY

    International Nuclear Information System (INIS)

    The principle of the proposed experiment is to irradiate very pure actinide samples in the Advanced Test Reactor (ATR) at INL and, after a given time, determine the amount of the different transmutation products. The determination of the nuclide densities before and after neutron irradiation will allow inference of effective neutron capture cross-sections. This approach has been used in the past and the novelty of this experiment is that the atom densities of the different transmutation products will be determined using the Accelerator Mass Spectroscopy (AMS) technique at the ATLAS facility located at ANL. It is currently planned to irradiate the following isotopes: 232Th, 235U, 236U, 238U, 237Np, 238Pu, 239Pu, 240Pu, 241Pu, 242Pu, 241Am, 243Am and 248Cm.

  19. Nanogram-scale preparation and NMR analysis for mass-limited small volatile compounds.

    Directory of Open Access Journals (Sweden)

    Satoshi Nojima

    Full Text Available Semiochemicals are often produced in infinitesimally small quantities, so their isolation requires large amounts of starting material, not only requiring significant effort in sample preparation, but also resulting in a complex mixture of compounds from which the bioactive compound needs to be purified and identified. Often, compounds cannot be unambiguously identified by their mass spectra alone, and NMR analysis is required for absolute chemical identification, further exacerbating the situation because NMR is relatively insensitive and requires large amounts of pure analyte, generally more than several micrograms. We developed an integrated approach for purification and NMR analysis of <1 µg of material. Collections from high performance preparative gas-chromatography are directly eluted with minimal NMR solvent into capillary NMR tubes. With this technique, (1H-NMR spectra were obtained on 50 ng of geranyl acetate, which served as a model compound, and reasonable H-H COSY NMR spectra were obtained from 250 ng of geranyl acetate. This simple off-line integration of preparative GC and NMR will facilitate the purification and chemical identification of novel volatile compounds, such as insect pheromones and other semiochemicals, which occur in minute (sub-nanogram, and often limited, quantities.

  20. Liquefaction of bio-mass in hot-compressed water for the production of phenolic compounds.

    Science.gov (United States)

    Tymchyshyn, Matthew; Xu, Chunbao Charles

    2010-04-01

    Direct liquefaction of lignocellulosic wastes (sawdust and cornstalks) and two model bio-mass compounds (pure lignin and pure cellulose as references) has been conducted in hot-compressed water at temperatures from 250 to 350 degrees C in the presence of 2MPa H(2), for the production of phenolic compounds that may be suitable for the production of green phenol-formaldehyde resins. The liquefaction operations at 250 degrees C for 60 min produced the desirable product of phenolic/neutral oil at a yield of about 53, 32, 32 and 17 wt.% for lignin, sawdust, cornstalk and cellulose, respectively. The yield of phenolic/neutral oil for each feedstock was found to decrease with increasing temperature. As evidenced by GC-MS measurements, significant quantities of phenolic compounds such as 2-methoxy-phenol, 4-ethyl-2-methoxy-phenol, and 2,6-dimethoxy-phenol, were present in the resulting phenolic/neutral oils from the two lignocellulosic wastes and pure lignin. The relative concentration of phenolic compounds in the lignin-derived oil was as high as about 80%. As expected, the liquid products from cellulose contained essentially carboxylic acids and neutral compounds. Addition of Ba(OH)(2) and Rb(2)CO(3) catalysts were found to significantly increase both phenolic/neutral oil and gas yields for all feedstocks except for lignin. PMID:20031393

  1. Small-size mass spectrometer for determining gases and volatile compounds in air during breathing

    Science.gov (United States)

    Kogan, V. T.; Kozlenok, A. V.; Chichagov, Yu. V.; Antonov, A. S.; Lebedev, D. S.; Bogdanov, A. A.; Moroshkin, V. S.; Berezina, A. V.; Viktorova-Leclerc, O. S.; Vlasov, S. A.; Tubol'tsev, Yu. V.

    2015-10-01

    We describe an automated mass spectrometer for diagnostics of deceases from the composition of exhaled air. It includes a capillary system, which performs a rapid direct feeding of the sample to the instrument without changing substantially its composition and serves for studying the dynamics of variation of the ratio between various components of exhaled air. The membrane system for introducing the sample is intended for determining low concentrations of volatile organic compounds which are biomarkers of pathologies. It is characterized by selective transmittance and ensures the detection limits of target compounds at the parts per million-parts per billion (ppm-ppb) level. A static mass analyzer operating on permanent magnets possesses advantages important for mobile devices as compared to its dynamic analogs: it is more reliable in operation, has a larger dynamic range, and can be used for determining the concentration of components in the mixture one-by-one or simultaneously. The curvilinear output boundary of the magnetic lens of the mass analyzer makes it possible to reduce its weight and size by 2.5 times without deteriorating the mass resolution. We report on the results of testing of the instrument and consider the possibility of its application for early detection of deceases of respiratory and blood circulation system, gastrointestinal tract, and endocrine system.

  2. MANTRA: Measuring Neutron Capture Cross Sections in Actinides with Accelerator Mass Spectrometry

    Science.gov (United States)

    Bauder, W.; Pardo, R. C.; Collon, P.; Palchan, T.; Scott, R.; Vondrasek, R.; Nusair, O.; Nair, C.; Paul, M.; Kondev, F.; Chen, J.; Youinou, G.; Salvatores, M.; Palmotti, G.; Berg, J.; Maddock, T.; Imel, G.

    2013-10-01

    With rising global energy needs, there is substantial interest in nuclear energy research. To explore possibilities for advanced fuel cycles, better neutron cross section data are needed for the minor actinides. The MANTRA (Measurement of Actinide Neutron TRAsmutation) project will improve these data by measuring integral (n, γ) cross sections. The cross sections will be extracted by measuring isotopic ratios in pure actinide samples, irradiated in the Advanced Test Reactor at Idaho National Lab, using Accelerator Mass Spectrometry(AMS) at the Argonne Tandem Linac Accelerator System (ATLAS). MANTRA presents a unique AMS challenge because of the goal to measure multiple isotopic ratios on a large number of samples. To meet these challenges, we have modified the AMS setup at ATLAS to include a laser ablation system for solid material injection into our ECR ion source. I will present work on the laser ablation system and modified source geometry, as well as preliminary measurements of unirradiated actinide samples at ATLAS. This work was supported by the U.S. Department of Energy, Office of Nuclear Physics, under Contract No. DE-AC02-06CH11357.

  3. Tidal capture formation of Low Mass X-Ray Binaries from wide binaries in the field

    CERN Document Server

    Michaely, Erez

    2015-01-01

    We present a potentially efficient dynamical formation scenario for Low Mass X-ray Binaries (LMXBs) in the field, focusing on black-hole (BH) LMXBs. In this formation channel LMXBs are formed from wide binaries $(>1000$ AU) with a BH component and a stellar companion. The wide binary is perturbed by fly-by's of field stars and its orbit random-walks and changes over time. This diffusion process can drive the binary into a sufficiently eccentric orbit such that the binary components tidally interact at peri-center and the binary evolves to become a short period binary, which eventually evolves into an LMXB. The formation rate of LMXBs through this channel mostly depends on the number of such BH wide binaries progenitors, which in turn depends on the velocity kicks imparted to BHs (or NSs) at birth. We consider several models for the formation and survival of such wide binaries, and calculate the LMXB formation rates for each model. We find that models where BHs form through direct collapse with no/little natal...

  4. Efficient mining of myxobacterial metabolite profiles enabled by liquid chromatography-electrospray ionisation-time-of-flight mass spectrometry and compound-based principal component analysis

    International Nuclear Information System (INIS)

    Bacteria producing secondary metabolites are an important source of natural products with highly diverse structures and biological activities. Developing methods to efficiently mine procaryotic secondary metabolomes for the presence of potentially novel natural products is therefore of considerable interest. Modern mass spectrometry-coupled liquid chromatography can effectively capture microbial metabolic diversity with ever improving sensitivity and accuracy. In addition, computational and statistical tools increasingly enable the targeted analysis and exploration of information-rich LC-MS datasets. In this article, we describe the use of such techniques for the characterization of myxobacterial secondary metabolomes. Using accurate mass data from high-resolution ESI-TOF measurements, target screening has facilitated the rapid identification of known myxobacterial metabolites in extracts from nine Myxococcus species. Furthermore, principal component analysis (PCA), implementing an advanced compound-based bucketing approach, readily revealed the presence of further compounds which contribute to variation among the metabolite profiles under investigation. The generation of molecular formulae for putative novel compounds with high confidence due to evaluation of both exact mass position and isotopic pattern, is exemplified as an important key for de-replication and prioritization of candidates for further characterization

  5. A Mass-Dependent Yield Origin of Neutron-Capture Element Abundance Distributions in Ultra-Faint Dwarfs

    CERN Document Server

    Lee, Duane M; Tumlinson, Jason; Sen, Bodhisattva; Simon, Joshua D

    2013-01-01

    One way to constrain the nature of the high-redshift progenitors of the Milky Way is to look at the low-metallicity stellar populations of the different Galactic components today. For example, high-resolution spectroscopy of very metal poor (VMP) stars demonstrates remarkable agreement between the distribution of [Ti/Fe] in the stellar populations of the Milky Way halo (MW) and ultra-faint dwarf (UFD) galaxies. In contrast, for the neutron capture (nc) abundance ratio distributions [(Sr,Ba)/Fe], the peak of the small UFD sample (6 stars) exhibits a signicant under-abundance relative to the VMP stars in the larger MW halo sample (~ 300 stars). We present a simple scenario that can simultaneously explain these similarities and differences by assuming: (i) that the MW VMP stars were predominately enriched by a prior generation of stars which possessed a higher total mass than the prior generation of stars that enriched the UFD VMP stars; and (ii) a much stronger mass-dependent yield (MDY) for nc-elements than fo...

  6. {sup 1}H and {sup 10}B NMR and MRI investigation of boron- and gadolinium-boron compounds in boron neutron capture therapy

    Energy Technology Data Exchange (ETDEWEB)

    Bonora, M., E-mail: marco.bonora@unipv.it [Physics Department ' A. Volta' , University of Pavia, Via Bassi 6, 27100 Pavia (Italy)] [CNISM Unit (Italy); Corti, M.; Borsa, F. [Physics Department ' A. Volta' , University of Pavia, Via Bassi 6, 27100 Pavia (Italy)] [CNISM Unit (Italy); Bortolussi, S.; Protti, N.; Santoro, D.; Stella, S.; Altieri, S. [Nuclear and Theoretical Physics Department, University of Pavia, Via Bassi 6, 27100 Pavia (Italy)] [INFN Pavia (Italy); Zonta, C.; Clerici, A.M.; Cansolino, L.; Ferrari, C.; Dionigi, P. [Surgical Sciences Department, Experimental Surgery Laboratory, University of Pavia, Pavia (Italy); Porta, A.; Zanoni, G.; Vidari, G. [Organic Chemistry Department, University of Pavia, Via Taramelli 10, 27100 Pavia (Italy)

    2011-12-15

    {sup 10}B molecular compounds suitable for Boron Neutron Capture Therapy (BNCT) are tagged with a Gd(III) paramagnetic ion. The newly synthesized molecule, Gd-BPA, is investigated as contrast agent in Magnetic Resonance Imaging (MRI) with the final aim of mapping the boron distribution in tissues. Preliminary Nuclear Magnetic Resonance (NMR) measurements, which include {sup 1}H and {sup 10}B relaxometry in animal tissues, proton relaxivity of the paramagnetic Gd-BPA molecule in water and its absorption in tumoral living cells, are reported.

  7. Storage ion trap of an 'In-Flight Capture' type for precise mass measurement of radioactive nuclear reaction products and fission fragments

    International Nuclear Information System (INIS)

    Data on nuclear masses provide a basis for creating and testing various nuclear models. A tandem system of FLNR comprised of the U-400M cyclotron, the COMBAS magnetic separator and the mass-spectrometric ion trap of an 'in-flight capture' type is considered as a possible complex for producing of the short-lived nuclei in fragmentation reactions by heavy ions and for precise mass measurement of these nuclei. The plan of scientific and technical FLNR research includes a project DRIBs for producing beams of accelerated radioactive nuclear reaction products and photofission fragments. This project proposes also precise mass measurements of the fission fragment with the help of the ion trap. The in-flight entrance of the ions and their capture in the mass-spectrometric ion trap using the monochromatizing degrader, the static electric and magnetic fields and a new invention, a magnetic unidirectional transporting ventil, is considered

  8. Headspace gas chromatography-mass spectrometry of volatile compounds in murici (Byrsonima crassifolia l. Rich).

    Science.gov (United States)

    Alves, G L; Franco, M R B

    2003-01-24

    Northern and Northeastern Brazil have a natural diversity of fruits, many of which are considered exotic, presenting different flavors and aromas. The enormous diversity of fruits represents a promising area for research on aromas. There is also a great potential for the manufacture of juices, desserts or other processed products. Murici is a typical fruit from these regions presenting a different flavor, reminiscent of that of cheese. This fruit is consumed mainly as juice, ice cream or as liquor, greatly appreciated by the local population. Headspace volatile compounds of three lots of the fruit from Ceará (Fortaleza) were collected by suction on Porapak Q for 2 h and desorbed with 300 microl of acetone. The isolated volatile compounds were separated by high resolution GC. Forty-six volatile compounds were detected, of which 41 were identified by gas chromatography-mass spectrometry and Kovats indices. The most abundant compounds were ethanol (28.3%) and ethyl hexanoate (25.1%). Butanoic acid (5.1%), hexanoic acid (5.1%) and methyl butyrate (2.8%) were also detected in the headspace of the fruit and confirm its unusual cheese aroma. PMID:12580497

  9. Real-time monitoring of volatile organic compounds using chemical ionization mass spectroscopy: Final report

    Energy Technology Data Exchange (ETDEWEB)

    Thornberg, S.M.; Mowry, C.D.; Keenan, M.R.; Bender, S.F.A. [Sandia National Labs., Albuquerque, NM (United States). Gas Analysis Lab.; Owen, T. [Intel Corp., Rio Rancho, NM (United States)

    1997-04-01

    Volatile organic compound (VOC) emission to the atmosphere is of great concern to semiconductor manufacturing industries, research laboratories, the public, and regulatory agencies. Some industries are seeking ways to reduce emissions by reducing VOCs at the point of use (or generation). This paper discusses the requirements, design, calibration, and use of a sampling inlet/quadrupole mass spectrometer system for monitoring VOCs in a semiconductor manufacturing production line. The system uses chemical ionization to monitor compounds typically found in the lithography processes used to manufacture semiconductor devices (e.g., acetone, photoresist). The system was designed to be transportable from tool to tool in the production line and to give the operator real-time feedback so the process(es) can be adjusted to minimize VOC emissions. Detection limits ranging from the high ppb range for acetone to the low ppm range fore other lithography chemicals were achieved using chemical ionization mass spectroscopy at a data acquisition rate of approximately 1 mass spectral scan (30 to 200 daltons) per second. A demonstration of exhaust VOC monitoring was performed at a working semiconductor fabrication facility during actual wafer processing.

  10. Understanding and controlling airborne organic compounds in the indoor environment: mass transfer analysis and applications.

    Science.gov (United States)

    Zhang, Y; Xiong, J; Mo, J; Gong, M; Cao, J

    2016-02-01

    Mass transfer is key to understanding and controlling indoor airborne organic chemical contaminants (e.g., VVOCs, VOCs, and SVOCs). In this study, we first introduce the fundamentals of mass transfer and then present a series of representative works from the past two decades, focusing on the most recent years. These works cover: (i) predicting and controlling emissions from indoor sources, (ii) determining concentrations of indoor air pollutants, (iii) estimating dermal exposure for some indoor gas-phase SVOCs, and (iv) optimizing air-purifying approaches. The mass transfer analysis spans the micro-, meso-, and macroscales and includes normal mass transfer modeling, inverse problem solving, and dimensionless analysis. These representative works have reported some novel approaches to mass transfer. Additionally, new dimensionless parameters such as the Little number and the normalized volume of clean air being completely cleaned in a given time period were proposed to better describe the general process characteristics in emissions and control of airborne organic compounds in the indoor environment. Finally, important problems that need further study are presented, reflecting the authors' perspective on the research opportunities in this area. PMID:25740682

  11. Modernization of Chinese herbal compound and the high performance liquid chromatography tandem mass spectrometry (HPLC-MS)

    Institute of Scientific and Technical Information of China (English)

    LI Wen-lan; SUN Zhi; DU Juan

    2008-01-01

    Chinese herbal compound is playing an important role on curing human diseases. And it has been a trend that Chinese herbal compound is being used all over the world in 21 century. However, our Chinese herbal compound is facing serious challenge for the lack of canonical system of quality criterion for Chinese herbal compound so it has been a urgent problem to set up the quality control standards and reveal therapeutic basis of Chinese herbal compound. In order to give full play to the advantages of Chinese herbal compound, modern scientific and technological is used to research of Chinese herbal compound, especially the high performance liquid chromatography tandem mass spectrometry(HPLC-MS), because it is high sensitive, rapid, and obtain more information. It is very necessary that HPLC-MS is uesed to elucidate the effective components of basic substances of Chinese Herbal Compound, and endow traditional Chinese medicine with modern scientific connotation.

  12. Boron-11 NMR spectroscopy of excised mouse tissues after infusion of boron compound used in neutron capture therapy

    International Nuclear Information System (INIS)

    Boron neutron capture therapy (BNCT) is based on selective boron uptake by the tumor and in situ activation by neutron beam. The authors propose the use of B-11 MR spectroscopy to noninvasively study boron uptake in animal tumor models. Sodium mercaptoundeca-hydrododecaborate was infused into female BALB/cJ mice and liver, brain, spleen, kidney, and tumor tissues were excised for MR (27.4MHz) and total boron content measurements. Boron-11 was easily detectable in tumor, liver, spleen, and skin. The results gave a very good correlation (correlation coefficient of .997) between B-11 MR measurements and total boron content of excised mouse tissues

  13. DETERMINATION OF CHEMICAL CLASSES FROM MASS SPECTRA OF TOXIC ORGANIC COMPOUNDS BY SIMCA PATTERN RECOGNITION AND INFORMATION THEORY

    Science.gov (United States)

    The low resolution mass spectra of a set of 78 toxic volatile organic compounds were examined for information concerning chemical classes. These compounds were predominately chloro- and/or bromoaromatics, -alkanes, or -alkenes, which are routinely sought at trace levels in ambien...

  14. A mass transfer model for predicting emission of the volatile organic compounds in wet building materials

    Institute of Scientific and Technical Information of China (English)

    ZHANG Tao; JIA Li

    2008-01-01

    A new mass transfer model is developped to predict the volatile organic compounds (VOCs) from fresh wet building materials. The dry section of wet materials during the process of VOC emission from wet building materials is considered in this new model, differing from the mass transfer-based models in other literatures. The mechanism of effect of saturated vapor pressure on the surface of wet building materials in the process of VOC emission is discussed. The concentration of total volatile organic compounds (TVOC) in the building materials gradually decreases as the emission of VOCs begins, and the vapor pressure of VOCs on the surface of wet building materials decreases in the case of newly wet building materials. To ensure the partial pressure of VOCs on the surface of wet building materials to be saturated vapor pressure, the interface of gas-wet layer is lowered, and a dry layer of no-volatile gases in the material is formed. Compared with the results obtained by VB model, CFD model and the ex-periment data, the results obtained by the present model agree well with the results obtained by CFD model and the experiment data. The present model is more accurate in predicting emission of VOC from wet building materials than VB model.

  15. Investigation of Spectra (NMR, Mass) of Some Fe3S3 Cluster Compounds

    Institute of Scientific and Technical Information of China (English)

    刘平; 王艰; 陈忠; 彭奇

    2000-01-01

    The chemical shifts of 1H-NMR of five Fe3S3 cluster compounds wereassigned. The main chemical shift values are: δcH3 = 1. 095 - 1. 946, δCH2 = 2. 882 -3.803, δC6Hn = 7. 547 7. 172. In comparison with those of pure (CH3CH2)3N andthiophenol, these values are moved to high position, and the width of these peaks is ob-viously increased. These characteristics conformed to NMR spectra of paramagneticcompounds and their molecular structures. The paramagnetic property of these com-pounds was also studied with ESR spectrum. Mass spectra of three compounds were de-termined. The main fragments were observed, for example, m/z: 130 [(C2H5)4N]+,264[Fe3S3] +, 144[Fe-S-Fe] +, 120[S-Fe-S]+, 88[Fe-S]+, 136[FeBr]+, 91[FeCl] + etc. These supported structural characteristics of the anion skeleton and molecules strongly. The possible mechanism of fragmentation was discussed.

  16. Photon mass attenuation coefficients, effective atomic numbers and electron densities of some thermoluminescent dosimetric compounds

    Indian Academy of Sciences (India)

    Shivalinge Gowda; S Krishnaveni; T Yashoda; T K Umesh; Ramakrishna Gowda

    2004-09-01

    Photon mass attenuation coefficients of some thermoluminescent dosimetric (TLD) compounds, such as LiF, CaCO3, CaSO4, CaSO4·2H2O, SrSO4, CdSO4, BaSO4, C4H6BaO4 and 3CdSO4·8H2O were determined at 279.2, 320.07, 514.0, 661.6, 1115.5, 1173.2 and 1332.5 keV in a well-collimated narrow beam good geometry set-up using a high resolution, hyper pure germanium detector. The attenuation coefficient data were then used to compute the effective atomic number and the electron density of TLD compounds. The interpolation of total attenuation cross-sections of photons of energy in elements of atomic number was performed using the logarithmic regression analysis of the data measured by the authors and reported earlier. The best-fit coefficients so obtained in the photon energy range of 279.2 to 320.07 keV, 514.0 to 661.6 keV and 1115.5 to 1332.5 keV by a piece-wise interpolation method were then used to find the effective atomic number and electron density of the compounds. These values are found to be in agreement with other available published values.

  17. Capillary gas chromatography-mass spectrometry of volatile and semi-volatile compounds of Salvia officinalis.

    Science.gov (United States)

    Radulescu, Valeria; Chiliment, Silvia; Oprea, Eliza

    2004-02-20

    The essential oil and infusion of Salvia officinalis leaves have been widely applied in traditional medicine since ancient times and nowadays subjected to extensive research of their antibacterial, antiviral and cytotoxic properties. This paper shows chemical composition data of S. officinalis leaves essential oil isolated by steam distillation using a Clevenger-type apparatus. Also, the paper presents the chemical content of volatile and semi-volatile compounds of S. officinalis leaves infusion. The volatile and semi-volatile compounds of S. officinalis leaves infusion were isolated by solid-phase extraction (SPE) and liquid-liquid extraction with hexane and dichloromethane. SPE was carried out on 500 mg octadecylsilane (C18) cartridges and elution with dichloromethane. Liquid-liquid extraction was performed with hexane and dichloromethane. The essential oil in dichloromethane and infusion extracts in hexane and dichloromethane were analyzed by gas chromatography coupled with mass spectrometry. The quantitative results obtained by solid-phase extraction and liquid-liquid extraction showed that SPE on C18 performed the highest recovery of the volatile compounds from infusion sample. PMID:14971492

  18. Electron capture dissociation and drift tube ion mobility-mass spectrometry coupled with site directed mutations provide insights into the conformational diversity of a metamorphic protein

    OpenAIRE

    Harvey, Sophie R.; Porrini, Massimiliano; Tyler, Robert C.; MacPhee, Cait E.; Volkman, Brian F.; Barran, Perdita E.

    2015-01-01

    Ion mobility mass spectrometry can be combined with data from top-down sequencing to discern adopted conformations of proteins in the absence of solvent. This multi-technique approach has particular applicability for conformationally dynamic systems. Previously, we demonstrated the use of drift tube ion mobility-mass spectrometry (DT IM-MS) and electron capture dissociation (ECD) to study the metamorphic protein lymphotactin (Ltn). Ltn exists in equilibrium between distinct monomeric (Ltn10) ...

  19. The Electron Capture Decay of 163-Ho to Measure the Electron Neutrino Mass with sub-eV Accuracy and Beyond

    CERN Document Server

    Gatti, Flavio; Lusignoli, Maurizio; Nucciotti, Angelo; Ragazzi, Stefano

    2012-01-01

    We have investigated the possibility of measuring the electron neutrino mass with sub-eV sensitivity by studying the electron capture decay of 163-Ho with cryogenic microcalorimeters. In this paper we will introduce an experiment's concept, discuss the technical requirements, and identify a roadmap to reach a sensitivity of 0.1 eV and beyond.

  20. Dereplication of Known Nucleobase and Nucleoside Compounds in Natural Product Extracts by Capillary Electrophoresis-High Resolution Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Junhui Chen

    2015-03-01

    Full Text Available Nucleobase and nucleoside compounds exist widely in various organisms. An often occurring problem in the discovery of new bioactive compounds from natural products is reisolation of known nucleobase and nucleoside compounds. To resolve this problem, a capillary electrophoresis-high resolution mass spectrometry (CE-HR-MS method providing both rapid separation and accurate mass full-scan MS data was developed for the first time to screen and dereplicate known nucleobase and nucleoside compounds in crude extracts of natural products. Instrumental parameters were optimized to obtain optimum conditions for CE separation and electrospray ionization-time-of-flight mass spectrometry (ESI-TOF/MS detection. The proposed method was verified to be precise, reproducible, and sensitive. Using this method, known nucleobase and nucleoside compounds in different marine medicinal organisms including Syngnathus acus Linnaeus; Hippocampus japonicus Kaup and Anthopleura lanthogrammica Berkly were successfully observed and identified. This work demonstrates that CE-HR-MS combined with an accurate mass database may be used as a powerful tool for dereplicating known nucleobase and nucleoside compounds in different types of natural products. Rapid dereplication of known nucleobase and nucleoside compounds allows researchers to focus on other leads with greater potential to yield new substances.

  1. Calculations of Compound Nucleus Spin-Parity Distributions Populated via the (p,t) Reaction in Support of Surrogate Neutron Capture Measurements

    Science.gov (United States)

    Benstead, J.; Tostevin, J. A.; Escher, J. E.; Burke, J. T.; Hughes, R. O.; Ota, S.; Casperson, R. J.; Thompson, I. J.

    2016-06-01

    The surrogate reaction method may be used to determine the cross section for neutron induced reactions not accessible through standard experimental techniques. This is achieved by creating the same compound nucleus as would be expected in the desired reaction, but through a different incident channel, generally a direct transfer reaction. So far, the surrogate technique has been applied with reasonable success to determine the fission cross section for a number of actinides, but has been less successful when applied to other reactions, e.g. neutron capture, due to a `spin-parity mismatch'. This mismatch, between the spin and parity distributions of the excited levels of the compound nucleus populated in the desired and surrogate channels, leads to differing decay probabilities and hence reduces the validity of using the surrogate method to infer the cross section in the desired channel. A greater theoretical understanding of the expected distribution of levels excited in both the desired and surrogate channels is therefore required in order to attempt to address this mismatch and allow the method to be utilised with greater confidence. Two neutron transfer reactions, e.g. (p,t), which allow the technique to be utilised for isotopes further removed from the line of stability, are the subject of this study. Results are presented for the calculated distribution of compound nucleus states populated in 90Zr, via the 90Zr(p,t)90Zr reaction, and are compared against measured data at an incident proton energy of 28.56 MeV.

  2. Characterization of volatile organic compounds by thermal desorption/gas chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Carbonaceous triple sorbent traps (TSTs) have been widely used to collect and concentrate volatile organic compounds (VOCs) in vapor phase samples for subsequent GC/MS analysis. Recently, this laboratory has been involved in sampling and analyzing VOCs collected from various emission sources, including headspace samples from underground storage tanks at the Department of Energy's Hanford site, in Richland, Washington. In order to evaluate the sampling adequacy and to assess any health-related impact based on the analysis results, a validated method must be employed. Therefore, the main objective of this study was to develop a methology for thermal desorption/gas chromatography/mass spectrometry (TD/GC/MS) determination of VOCs in the vapor phase samples collected on Carbotrap C/Carbotrap/Carbosieve S III triple sorbent traps. Techniques used in method validation included VOC standard generation, thermal desorption efficiency, reproducibility of spiking on and recovery from TST, use of internal standards, detection limits determination, linearity and reproducibility of calibration

  3. [Determination of 10 volatile organic compounds in toys by headspace gas chromatography-mass spectrometry].

    Science.gov (United States)

    Lü, Qing; Zhang, Qing; Kang, Suyuan; Bai, Hua; Wang, Chao

    2010-08-01

    A headspace gas chromatography-mass spectrometry (HS-GC-MS) method was developed for the determination of 10 residual volatile organic compounds (VOCs) in toys. The experimental conditions such as headspace temperature, headspace time and the analytical conditions of GC-MS were optimized. Toy samples were treated at 140 degrees C for 45 min, and then the evolved products were separated on a DB-624 column, determined by MS and quantified by external standard method. The recoveries were from 79% to 106% and the relative standard deviations (RSDs) were from 0.4% to 5.6%. The linear range was 0.001 - 2.0 microg with a good linear correlation coefficient (r > 0.994 0) and the limits of quantification (LOQ) were less than 0 66 mg/kg. The method is accurate, simple, rapid, and is suitable for the analysis of residual VOCs in various toys. PMID:21261051

  4. Characterization of sulfur compounds in supercritical coal extracts by gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Gryglewicz, Grazyna; Rutkowski, Piotr [Institute of Chemistry and Technology of Petroleum and Coal, Wroclaw University of Technology, ul. Gdanska 7/9, 50-344 Wroclaw (Poland); Yperman, Jan [Laboratory of Applied Chemistry, IMO, Limburgs Universitair Centrum, Universiteitslaan, B-3590 Diepenbeek (Belgium)

    2002-06-20

    The organosulfur compounds (OSC) in the supercritical extracts obtained from flame coal (subA) and orthocoking coal (mvb) were identified by gas chromatography-mass spectrometry. Supercritical fluid extraction was carried out with three different solvents, i.e., toluene, toluene/2-propanol and toluene/THF mixtures, at 360 C and 10 MPa in an apparatus with continuous flow of solvent. The extraction yield was in the range of 11.4-39.9 wt.% depending on the type of solvent and coal. For flame coal, diphenyl sulfide and disulfide, thiophene, benzothiophene, dibenzothiophene and benzonaphtothiophene and their C{sub 1}-C{sub 4} alkyl derivatives were detected, whereas for orthocoking coal only polycyclic aromatic sulfur heterocycles (PASH) containing two to five rings and their alkyl derivatives were found. Ligand exchange chromatography was applied to separate the PASH fraction.

  5. Mass flows of perfluorinated compounds (PFCs) in central wastewater treatment plants of industrial zones in Thailand.

    Science.gov (United States)

    Kunacheva, Chinagarn; Tanaka, Shuhei; Fujii, Shigeo; Boontanon, Suwanna Kitpati; Musirat, Chanatip; Wongwattana, Thana; Shivakoti, Binaya Raj

    2011-04-01

    Perfluorinated compounds (PFCs) are fully fluorinated organic compounds, which have been used in many industrial processes and have been detected in wastewater and sludge from municipal wastewater treatment plants (WWTPs) around the world. This study focused on the occurrences of PFCs and PFCs mass flows in the industrial wastewater treatment plants, which reported to be the important sources of PFCs. Surveys were conducted in central wastewater treatment plant in two industrial zones in Thailand. Samples were collected from influent, aeration tank, secondary clarifier effluent, effluent and sludge. The major purpose of this field study was to identify PFCs occurrences and mass flow during industrial WWTP. Solid-phase extraction (SPE) coupled with HPLC-ESI-MS/MS were used for the analysis. Total 10 PFCs including perfluorooctane sulfonate (PFOS), perfluorooctanoic acid (PFOA), perfluoropropanoic acid (PFPA), perfluorohexanoic acid (PFHxA), perfluoroheptanoic acid (PFHpA), perfluorohexane sulfonate (PFHxS), perfluoronanoic acid (PFNA), perfluordecanoic acid (PFDA), perfluoroundecanoic acid (PFUnA), and perfluorododecanoic acid (PFDoA) were measured to identify their occurrences. PFCs were detected in both liquid and solid phase in most samples. The exceptionally high level of PFCs was detected in the treatment plant of IZ1 and IZ2 ranging between 662-847ngL(-1) and 674-1383ngL(-1), respectively, which greater than PFCs found in most domestic wastewater. Due to PFCs non-biodegradable property, both WWTPs were found ineffective in removing PFCs using activated sludge processes. Bio-accumulation in sludge could be the major removal mechanism of PFCs in the process. The increasing amount of PFCs after activated sludge processes were identified which could be due to the degradation of PFCs precursors. PFCs concentration found in the effluent were very high comparing to those in river water of the area. Industrial activity could be the one of major sources of PFCs

  6. Study of the interaction of boron-containing amino acids for the neutron capture therapy with biologically interesting compounds by using 'three-spot zone electrophoresis'

    International Nuclear Information System (INIS)

    As the boron carriers for boron neutron capture therapy, p-borono phenylalanine (BPA) is the boron compound which has been clinically used together with sodium borocaptate. It was found by the electrophoresis behavior that the BPA interacted with organic carboxylic acids in its dissolved state. In this paper, the electrophoresis behavior of general amino acids as seen in three-spot zone electrophoresis and the peculiar interaction of the amino acids having dihydroxyboryl radical are described. Zone electrophoresis has been developed as separation means, and three-spot process excludes the errors due to accidental factors as far as possible. The behaviors of zone electrophoresis of ordinary neutral amino acids, orthoboric acid and p-BPA are reported. For utilizing the features of boron neutron capture therapy, it is necessary to develop the carrier which is singularly taken into cancer cells. There is not a good method for discriminating normal cells and cancer cells. As for the administration of BPA to patients, its solubility is insufficient, therefore, its fructose complex has been used. The research on the biochemical peculiarity of boron is important. (K.I.)

  7. ANALYSIS OF CHEMICAL COMPOUNDS OF AGARWOOD OIL FROM DIFFERENT SPECIES BY GAS CHROMATOGRAPHY MASS SPECTROMETRY (GCMS

    Directory of Open Access Journals (Sweden)

    Yumi Zuhanis Has-Yun Hashim

    2014-05-01

    Full Text Available ABSTRACT: Agarwood oil is a highly prized type of oil due to its unique aroma. The oil is extracted from the fragrant resin found in the agarwood tree (trunk.  The unique aroma and quality of agarwood resin and oil are contributed by the presence of certain chemical compounds. In this work, analysis and comparison of the chemical compounds of agarwood oil from A. malaccensis, A. sub-integra and a mixture of both were conducted.  The essential oils were diluted in hexane (5% prior to gas chromatography mass spectrometry (GCMS analysis performed using Agilent GCMS 7890A coupled with MSD quadrupole detector 5975 C.  Separation of analytes by gas chromatography was carried out using a Hewlett Packard HP-5MS silica capillary column (30 m X 0.25 mm X 0.25 mm. A total of 107 compounds were identified from the three samples of agarwood oils. Fifty-five (55 components were identified in A. malaccensis sample which contributes to the largest portion of the total compounds. About 20% of the compounds identified were aromatic and sesquiterpenes which have been revealed to be the main active compounds of agarwood oils which also give the aroma and pleasant odour of agarwood. Different compositions or profile of chemical components were found in agarwood oils from the two different species. Two compounds were commonly identified in all three samples namely 3-phenyl-2-butanone and alpha-cubebene.  Further studies are needed to refine the results which later can be used to assist detection and authentication of agarwood as well as its scientific-based grading. ABSTRAK: Minyak gaharu merupakan sejenis minyak beraroma unik yang mendapat permintaan tinggi dan mahal. Minyak ini diekstrak daripada resin beraroma yang terbentuk di dalam batang pokok gaharu. Keunikan aroma dan kualiti resin dan minyak gaharu ini bergantung kepada kehadiran bahan kimia tertentu. Penyelidikan ini menjurus kepada analisis dan perbandingan bahan-bahan kimia yang terdapat dalam minyak

  8. Using Mass Spectrometry to Detect Silanol Compounds in Water from the International Space Station

    Science.gov (United States)

    Rutz, Jeffrey A.; Kuo, C. K. Mike; Alverson, James T.; Wallace, William T.; Gazda, Daniel B.

    2016-01-01

    The water produced by the U.S. Water Processor Assembly (WPA) on the International Space Station had virtually undetectable levels of total organic carbon (TOC) during the first 18 months of operation. In 2010, the TOC in the WPA product water rose to approx. 2 mg/L. The maximum allowable TOC concentration in the product water is 3.0 mg/L. Ground analysis indicated that > 90% of this increase was due to dimethylsilanediol (DMSD). Since then, recurring increases in TOC attributed to DMSD have occurred every 12-18 months. In 2015, a new compound was determined to be responsible for the TOC increase. This new contaminant was identified as monomethylsilanetriol (MMST). This poster details the efforts to identify and quantify DMSD and MMST. DMSD was initially discovered as a stray peak in a routine GC/MS analysis used to measure glycols. This method was not suitable for routine analysis of DMSD because of extreme carryover problems. MMST was discovered and identified using direct infusion electrospray ionization (ESI) mass spectrometry. The identification was confirmed by purchasing an MMST standard and analyzing it by HPLC with refractive index (RI) detection. An LC/MS method has been developed, based on the LC/RI method that quantifies both DMSD and MMST in a 14-minute isocratic run. This method employs atmospheric pressure chemical ionization (APCI) and a single quadrupole mass spectrometer operated in negative mode with selected ion monitoring.

  9. Tandem Mass Spectrometry Measurement of the Collision Products of Carbamate Anions Derived from CO2 Capture Sorbents: Paving the Way for Accurate Quantitation

    Science.gov (United States)

    Jackson, Phil; Fisher, Keith J.; Attalla, Moetaz Ibrahim

    2011-08-01

    The reaction between CO2 and aqueous amines to produce a charged carbamate product plays a crucial role in post-combustion capture chemistry when primary and secondary amines are used. In this paper, we report the low energy negative-ion CID results for several anionic carbamates derived from primary and secondary amines commonly used as post-combustion capture solvents. The study was performed using the modern equivalent of a triple quadrupole instrument equipped with a T-wave collision cell. Deuterium labeling of 2-aminoethanol (1,1,2,2,-d4-2-aminoethanol) and computations at the M06-2X/6-311++G(d,p) level were used to confirm the identity of the fragmentation products for 2-hydroxyethylcarbamate (derived from 2-aminoethanol), in particular the ions CN-, NCO- and facile neutral losses of CO2 and water; there is precedent for the latter in condensed phase isocyanate chemistry. The fragmentations of 2-hydroxyethylcarbamate were generalized for carbamate anions derived from other capture amines, including ethylenediamine, diethanolamine, and piperazine. We also report unequivocal evidence for the existence of carbamate anions derived from sterically hindered amines ( Tris(2-hydroxymethyl)aminomethane and 2-methyl-2-aminopropanol). For the suite of carbamates investigated, diagnostic losses include the decarboxylation product (-CO2, 44 mass units), loss of 46 mass units and the fragments NCO- ( m/z 42) and CN- ( m/z 26). We also report low energy CID results for the dicarbamate dianion (-O2CNHC2H4NHCO{2/-}) commonly encountered in CO2 capture solution utilizing ethylenediamine. Finally, we demonstrate a promising ion chromatography-MS based procedure for the separation and quantitation of aqueous anionic carbamates, which is based on the reported CID findings. The availability of accurate quantitation methods for ionic CO2 capture products could lead to dynamic operational tuning of CO2 capture-plants and, thus, cost-savings via real-time manipulation of solvent

  10. Capturing Thoughts, Capturing Minds?

    DEFF Research Database (Denmark)

    Nielsen, Janni

    2004-01-01

    Think Aloud is cost effective, promises access to the user's mind and is the applied usability technique. But 'keep talking' is difficult, besides, the multimodal interface is visual not verbal. Eye-tracking seems to get around the verbalisation problem. It captures the visual focus of attention....... However, it is expensive, obtrusive and produces huge amount of data. Besides, eye-tracking do not give access to user's mind. Capturing interface/cursor tracking may be cost effective. It is easy to install, data collection is automatic and unobtrusive and replaying the captured recording to the user and...

  11. Effect of a new matrix system for low-polar organic compounds in fast atom bombardment mass spectrometry

    International Nuclear Information System (INIS)

    A new matrix system m-NBA-DTDE (1:1) for FABMS of low-polar compounds, such as cholesterol and stearic acid methyl ester, was prepared. The system, i.e., a 1:1 mixture of m-NBA (m-nitrobenzyl alcohol) to DTDE (2,2-dithiodiethanol or 2-hydroxyethyl disulfide), contributed to measuring the positive ion FAB mass spectra of above compounds and morusin permethyl ether, and it brought an effective result on the ion current lifetime and the reproducibility of their spectra. The positive ion FAB mass spectra of these low-polar compounds were compared with the corresponding positive ion EI and CI mass spectra. (author)

  12. Characterization of phenolic compounds using separation techniques coupled to mass spectrometry of plant extracts with demonstrated bioactivity

    OpenAIRE

    Iswaldi, Ihsan

    2012-01-01

    This doctoral thesis, entitled "Characterization of phenolic compounds using separation techniques coupled to mass spectrometry of plant extracts with demonstrated bioactivity", consists of two main sections: the Introduction and the Experimental Section. The first section describes an overview of traditional medicine and functional food, plant foods as natural source of bioactive compounds, polyphenols and bioactivity and the analytical tools used to identify polyphenols such as high-pe...

  13. Investigation of the mass loss of water soluble ionic compounds caused by EDXRF analysis of PM10 loaded filters

    Science.gov (United States)

    Yatkin, S.; Gerboles, M.

    2013-07-01

    The mass loss of particulate matter (PM) due to EDXRF analysis was gravimetrically evaluated on co-located PM10 loaded filters analyzed both using EDXRF under vacuum and using Ion Chromatography. Then, this comparison was repeated with air and helium (He) instead of evacuating the measurements chamber of the EDXRF spectrometer. It was shown that EDXRF application using vacuum medium led to mass loss of water soluble ionic compounds and other volatile constituents of PM10. The use of a He and air medium considerably reduced the PM mass losses. It is demonstrated that the mass loss of PM and ionic compounds mainly resulted from vacuum medium and from a lower extent to the level of X-ray energy. The influence of EDXRF application using vacuum medium on the mass losses of ionic compounds were further investigated. Different amounts of NO3-, NH4+, Cl-, Na+, Mg++ and Ca++ were lost whereas SO4-- and K+ remained unchanged. The relationship between vacuum and application time was also studied for quartz and Teflon filters. The longer the application time, the higher the PM mass loss was observed. The mass loss of PM on quartz filter was shown by experiments to be 2 times higher than on Teflon filter.

  14. Direct Measurement of Intracellular Compound Concentration by RapidFire Mass Spectrometry Offers Insights into Cell Permeability.

    Science.gov (United States)

    Gordon, Laurie J; Allen, Morven; Artursson, Per; Hann, Michael M; Leavens, Bill J; Mateus, André; Readshaw, Simon; Valko, Klara; Wayne, Gareth J; West, Andy

    2016-02-01

    One of the key challenges facing early stage drug discovery is understanding the commonly observed difference between the activity of compounds in biochemical assays and cellular assays. Traditionally, indirect or estimated cell permeability measurements such as estimations from logP or artificial membrane permeability are used to explain the differences. The missing link is a direct measurement of intracellular compound concentration in whole cells. This can, in some circumstances, be estimated from the cellular activity, but this may also be problematic if cellular activity is weak or absent. Advances in sensitivity and throughput of analytical techniques have enabled us to develop a high-throughput assay for the measurement of intracellular compound concentration for routine use to support lead optimization. The assay uses a RapidFire-MS based readout of compound concentration in HeLa cells following incubation of cells with test compound. The initial assay validation was performed by ultra-high performance liquid chromatography tandem mass spectrometry, and the assay was subsequently transferred to RapidFire tandem mass spectrometry. Further miniaturization and optimization were performed to streamline the process, increase sample throughput, and reduce cycle time. This optimization has delivered a semi-automated platform with the potential of production scale compound profiling up to 100 compounds per day. PMID:26336900

  15. Fundamental mass transfer modeling of emission of volatile organic compounds from building materials

    Science.gov (United States)

    Bodalal, Awad Saad

    In this study, a mass transfer theory based model is presented for characterizing the VOC emissions from building materials. A 3-D diffusion model is developed to describe the emissions of volatile organic compounds (VOCs) from individual sources. Then the formulation is extended to include the emissions from composite sources (system comprising an assemblage of individual sources). The key parameters for the model (The diffusion coefficient of the VOC in the source material D, and the equilibrium partition coefficient k e) were determined independently (model parameters are determined without the use of chamber emission data). This procedure eliminated to a large extent the need for emission testing using environmental chambers, which is costly, time consuming, and may be subject to confounding sink effects. An experimental method is developed and implemented to measure directly the internal diffusion (D) and partition coefficients ( ke). The use of the method is illustrated for three types of VOC's: (i) Aliphatic Hydrocarbons, (ii) Aromatic Hydrocarbons and ( iii) Aldehydes, through typical dry building materials (carpet, plywood, particleboard, vinyl floor tile, gypsum board, sub-floor tile and OSB). Then correlations for predicting D and ke based solely on commonly available properties such as molecular weight and vapour pressure were proposed for each product and type of VOC. These correlations can be used to estimate the D and ke when direct measurement data are not available, and thus facilitate the prediction of VOC emissions from the building materials using mass transfer theory. The VOC emissions from a sub-floor material (made of the recycled automobile tires), and a particleboard are measured and predicted. Finally, a mathematical model to predict the diffusion coefficient through complex sources (floor adhesive) as a function of time was developed. Then this model (for diffusion coefficient in complex sources) was used to predict the emission rate from

  16. Lunar Sulfur Capture System

    Science.gov (United States)

    Berggren, Mark; Zubrin, Robert; Bostwick-White, Emily

    2013-01-01

    The Lunar Sulfur Capture System (LSCS) protects in situ resource utilization (ISRU) hardware from corrosion, and reduces contaminant levels in water condensed for electrolysis. The LSCS uses a lunar soil sorbent to trap over 98 percent of sulfur gases and about two-thirds of halide gases evolved during hydrogen reduction of lunar soils. LSCS soil sorbent is based on lunar minerals containing iron and calcium compounds that trap sulfur and halide gas contaminants in a fixed-bed reactor held at temperatures between 250 and 400 C, allowing moisture produced during reduction to pass through in vapor phase. Small amounts of Earth-based polishing sorbents consisting of zinc oxide and sodium aluminate are used to reduce contaminant concentrations to one ppm or less. The preferred LSCS configuration employs lunar soil beneficiation to boost concentrations of reactive sorbent minerals. Lunar soils contain sulfur in concentrations of about 0.1 percent, and halogen compounds including chlorine and fluorine in concentrations of about 0.01 percent. These contaminants are released as gases such as H2S, COS, CS2,HCl, and HF during thermal ISRU processing with hydrogen or other reducing gases. Removal of contaminant gases is required during ISRU processing to prevent hardware corrosion, electrolyzer damage, and catalyst poisoning. The use of Earth-supplied, single-use consumables to entirely remove contaminants at the levels existing in lunar soils would make many ISRU processes unattractive due to the large mass of consumables relative to the mass of oxygen produced. The LSCS concept of using a primary sorbent prepared from lunar soil was identified as a method by which the majority of contaminants could be removed from process gas streams, thereby substantially reducing the required mass of Earth-supplied consumables. The LSCS takes advantage of minerals containing iron and calcium compounds that are present in lunar soil to trap sulfur and halide gases in a fixedbed reactor

  17. Natural compounds involved in adipose tissue mass control in in vitro studies

    Directory of Open Access Journals (Sweden)

    Katarzyna Kowalska

    2011-08-01

    Full Text Available The World Health Organization (WHO has recognized obesity as an epidemic of the 21st century. Obesity is pathological fat accumulation in the body influenced by many factors: metabolic, endocrine, genetic, environmental, psychological and behavioral. The quality and quantity of food intake to a considerable degree determine excessive fat accumulation in the body. The strategy in obesity prevention includes, among other things, a proper diet. It is widely known that a diet rich in fruits and vegetables reduces body weight. Adipocytes are not only cells serving as storage depots for “energy”, but are also specialized cells influenced by various hormones, cytokines and nutrients, which have pleiotropic effects on the body. Knowledge of adipocyte biology is crucial for our understanding of the pathophysiological basis of obesity and metabolic diseases, such as type 2 diabetes. Furthermore, rational manipulation of adipose physiology is a promising avenue for therapy of these conditions. Adipose tissue mass can be reduced through elimination of adipocytes by apoptosis, inhibition of adipogenesis and increased lipolysis in adipocytes. Natural products have a potential to induce apoptosis, inhibit adipogenesis and stimulate lipolysis in adipocytes. Various dietary bioactive compounds target different stages of the adipocyte life cycle and may be useful as natural therapeutic agents in obesity prevention.

  18. Temperature-dependent release of volatile organic compounds of eucalypts by direct analysis in real time (DART) mass spectrometry.

    Science.gov (United States)

    Maleknia, Simin D; Vail, Teresa M; Cody, Robert B; Sparkman, David O; Bell, Tina L; Adams, Mark A

    2009-08-01

    A method is described for the rapid identification of biogenic, volatile organic compounds (VOCs) emitted by plants, including the analysis of the temperature dependence of those emissions. Direct analysis in real time (DART) enabled ionization of VOCs from stem and leaf of several eucalyptus species including E. cinerea, E. citriodora, E. nicholii and E. sideroxylon. Plant tissues were placed directly in the gap between the DART ionization source skimmer and the capillary inlet of the time-of-flight (TOF) mass spectrometer. Temperature-dependent emission of VOCs was achieved by adjusting the temperature of the helium gas into the DART ionization source at 50, 100, 200 and 300 degrees C, which enabled direct evaporation of compounds, up to the onset of pyrolysis of plant fibres (i.e. cellulose and lignin). Accurate mass measurements facilitated by TOF mass spectrometry provided elemental compositions for the VOCs. A wide range of compounds was detected from simple organic compounds (i.e. methanol and acetone) to a series of monoterpenes (i.e. pinene, camphene, cymene, eucalyptol) common to many plant species, as well as several less abundant sesquiterpenes and flavonoids (i.e. naringenin, spathulenol, eucalyptin) with antioxidant and antimicrobial properties. The leaf and stem tissues for all four eucalypt species showed similar compounds. The relative abundances of methanol and ethanol were greater in stem wood than in leaf tissue suggesting that DART could be used to investigate the tissue-specific transport and emissions of VOCs. PMID:19551840

  19. Rapid in situ identification of bioactive compounds in plants by in vivo nanospray high-resolution mass spectrometry.

    Science.gov (United States)

    Chang, Qing; Peng, Yue'e; Dan, Conghui; Shuai, Qin; Hu, Shenghong

    2015-03-25

    A method for the rapid in situ identification of bioactive compounds in fresh plants has been developed using in vivo nanospray coupled to high-resolution mass spectrometry (HR-MS). Using a homemade in vivo nanospray ion source, the plant liquid was drawn out from a target region and ionized in situ. The ionized bioactive compounds were then identified using Q-Orbitrap HR-MS. The accurate mass measurements of these bioactive compounds were performed by full-scan or selected ion monitoring (SIM), and tandem mass spectrometry (MS/MS) was used in the structural elucidation. Without sample pretreatment, 12 bioactive compounds in 7 different plant species were identified, namely, isoalliin in onion; butylphthalide in celery; N-methylpelletierine, pelletierine, and pseudopelletierine in pomegranate; chlorogenic acid in crabapple; solamargine, solasonine, and solasodine in nightshade; aloin and aloe-emodin in aloe; and menthone in mint. This work demonstrates that in vivo nanospray HR-MS is a good method for rapid in situ identification of bioactive compounds in plants. PMID:25749134

  20. Expert system for estimates of molecular weights of volatile organic compounds from low-resolution mass spectra

    Energy Technology Data Exchange (ETDEWEB)

    Scott, D.R.

    1991-01-01

    MAXMASS, the highest mass with an intensity of 5% of the base peak in a low resolution mass spectrum, has been found to be linearly correlated with the true molecular weights of 400 randomly selected spectra, yielding a family of parellel lines. A simple expert system using MAXMASS has been developed to estimate molecular weights of unknown volatile compounds from their mass spectra. This is an empirical rule-based system which will run on a personal computer. It consists of a classification module chained to separate molecular weight prediction modules for six classes. These are benzenes; chlorobenzenes; bromoalkenes/alkenes; mono- and dichloroalkanes/alkenes; tri-, tetra- and pentachloroalkanes/alkenes; and unknown (other) classes. The rules were derived from National Institute of Standards and Technology (NIST) reference spectra of 75 target toxic compounds from the first five classes and 32 from the unknown class. Performance tests of molecular weight predictions were made with the expert system and the Self Training interpretive and Retrieval System (STIRS) on NIST reference spectra of the 107 training compounds; on a set of 32 test NIST reference spectra of other compounds found in air samples; on a set of 100 randomly selected NIST reference spectra; and on 30 spectra taken from actual field gas chromatography/mass spectrometry samples.

  1. Selected Ion Flow Tube-Mass Spectrometry for Absolute Quantification of Aroma Compounds in the Headspace of Dry Fermented Sausages

    Czech Academy of Sciences Publication Activity Database

    Olivares, A.; Dryahina, Kseniya; Navarro, J. L.; Flores, M.; Smith, D.; Španěl, Patrik

    2010-01-01

    Roč. 82, č. 13 (2010), s. 5819-5829. ISSN 0003-2700 R&D Projects: GA ČR GA203/09/0256 Institutional research plan: CEZ:AV0Z40400503 Keywords : mass spectrometry * aroma compounds * dry fermented sausages Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 5.874, year: 2010

  2. Reaction of low-molecular-mass organoselenium compounds (and their sulphur analogues) with inflammation-associated oxidants

    DEFF Research Database (Denmark)

    Carroll, L.; Davies, Michael J.; Pattison, D. I.

    2015-01-01

    the chemistry of low-molecular-mass organoselenium compounds (e.g. selenoethers, diselenides and selenols) with inflammatory oxidants, with a particular focus on the reaction kinetics and product studies, with the differences in reactivity between selenium and sulphur analogues described in the...

  3. Capillary electrophoresis-electrospray mass spectrometry and HR-ICP-MS for the detection and quantification of 10B-boronophenylalanine (10B-BPA) used in boron neutron capture therapy.

    Science.gov (United States)

    Pitois, Aurélien; de las Heras, Laura Aldave; Zampolli, Antonella; Menichetti, Luca; Carlos, Ramon; Lazzerini, Guido; Cionini, Luca; Salvatori, Pietro Alberto; Betti, Maria

    2006-02-01

    Boron neutron capture therapy (BNCT) is a bimodal radiotherapeutic treatment based on the irradiation of neoplastic tissues with neutrons after the tissues have selectively accumulated molecules loaded with nuclides with large neutron capture cross-sections (such boron-10). Boron-10 carriers have been tested to a limited extent, and clinical trials have been conducted on sulfhydryl borane (10B-BSH) and boronophenylalanine (10B-BPA). However, precise and accurate measurements of boron-10 concentrations (0.1-100 microg/g) in specimens and samples of limited size (microg scale) are needed in order to be able to biologically characterise new compounds in predictive tissue dosimetry, toxicology and pharmacology studies as well as in clinical investigations. A new approach based on fast separation and detection of 10B-BPA performed by coupling capillary electrophoresis to electrospray mass spectrometry is reported. This method allows the quantitative analysis and characterisation of 10B-BPA in a short time with a high separation efficiency. Detection limits of 3 microM for 10B-BPA and 30 ng/mL for 10B were obtained with CE-ESI-MS. A quantification limit of 10 microM for 10B-BPA (100 ng/mL for 10B) was attained. The total boron-10 concentration was determined by high-resolution inductively coupled mass spectrometry in order to validate the method. Boron-10 isotope measurements were carried out by HR-ICP-MS at medium resolution (R=4000) due to the presence of an isobaric interference at mass 10. Good agreement was obtained between the values from CE-ESI-MS and those from HR-ICP-MS. The method has been successfully used to determine the 10B-BPA in two lines of cultured cells. PMID:16372182

  4. Analysis of pharmaceutical and other organic wastewater compounds in filtered and unfiltered water samples by gas chromatography/mass spectrometry

    Science.gov (United States)

    Zaugg, Steven D.; Phillips, Patrick J.; Smith, Steven G.

    2014-01-01

    Research on the effects of exposure of stream biota to complex mixtures of pharmaceuticals and other organic compounds associated with wastewater requires the development of additional analytical capabilities for these compounds in water samples. Two gas chromatography/mass spectrometry (GC/MS) analytical methods used at the U.S. Geological Survey National Water Quality Laboratory (NWQL) to analyze organic compounds associated with wastewater were adapted to include additional pharmaceutical and other organic compounds beginning in 2009. This report includes a description of method performance for 42 additional compounds for the filtered-water method (hereafter referred to as the filtered method) and 46 additional compounds for the unfiltered-water method (hereafter referred to as the unfiltered method). The method performance for the filtered method described in this report has been published for seven of these compounds; however, the addition of several other compounds to the filtered method and the addition of the compounds to the unfiltered method resulted in the need to document method performance for both of the modified methods. Most of these added compounds are pharmaceuticals or pharmaceutical degradates, although two nonpharmaceutical compounds are included in each method. The main pharmaceutical compound classes added to the two modified methods include muscle relaxants, opiates, analgesics, and sedatives. These types of compounds were added to the original filtered and unfiltered methods largely in response to the tentative identification of a wide range of pharmaceutical and other organic compounds in samples collected from wastewater-treatment plants. Filtered water samples are extracted by vacuum through disposable solid-phase cartridges that contain modified polystyrene-divinylbenzene resin. Unfiltered samples are extracted by using continuous liquid-liquid extraction with dichloromethane. The compounds of interest for filtered and unfiltered sample

  5. Determination of some volatile compounds in alcoholic beverage by headspace solid-phase microextraction gas chromatography - mass spectrometry

    Science.gov (United States)

    Schmutzer, G.; Avram, V.; Feher, I.; David, L.; Moldovan, Z.

    2012-02-01

    The volatile composition of alcoholic beverage was studied by headspace solid-phase microextraction (HSSPME) method and gas chromatography - mass spectrometry (GC-MS). Some volatile compounds, such as alcohols, esters, terpenes and other are mainly responsible for the flavor of fortified wines and their amounts specify the quality of the alcoholic beverages. From this perspective it is interesting to develop a rapid, selective and sensitive analytical method suitable for simultaneous quantification of the main molecules being responsible for the organoleptic characteristic of alcoholic beverages. Vermouth fortified drink was analyzed in order to characterize the volatile profile. Using the HS-SPME/GC-MS a number of twenty-six volatile compounds from a commercial market alcoholic beverage were identified. The most abundant compounds were m-thymol, o-thymol and eugenol, alongside of the ethyl ester compounds.

  6. Determination of the effective atomic and mass numbers for mixture and compound materials in high energy photon interactions

    International Nuclear Information System (INIS)

    In consideration the radiological properties of materials and studying the scattering processes in atomic and nuclear physics, the effective atomic and mass numbers is widely employed. These numbers have been calculated for any mixed or composite materials in interaction with high energy photons (Linac in radiation therapy). A pair equation in terms of these numbers is obtained. The first equation has been derived from the conservation of mass energy law and the second by minimizing the binding energy from the semiempirical mass formula (Myers and Swiatecki formula) that gives a relation between atomic and mass numbers for stable nuclei approximately. By these equations one can obtain the effective atomic and mass numbers for any compound or mixed materials uniquely. These numbers are calculated for some materials and compared with the other studies. (author)

  7. Multiclass semi-volatile compounds determination in wine by gas chromatography accurate time-of-flight mass spectrometry.

    Science.gov (United States)

    Rodríguez-Cabo, T; Rodríguez, I; Ramil, M; Silva, A; Cela, R

    2016-04-15

    The performance of gas chromatography (GC) with accurate, high resolution mass spectrometry (HRMS) for the determination of a group of 39 semi-volatile compounds related to wine quality (pesticide residues, phenolic off-flavours, phenolic pollutants and bioactive stilbenes) is investigated. Solid-phase extraction (SPE) was used as extraction technique, previously to acetylation (phenolic compounds) and dispersive liquid-liquid microextraction (DLLME) concentration. Compounds were determined by GC coupled to a quadrupole time-of-flight (QTOF) MS system through an electron ionization (EI) source. The final method attained limits of quantification (LOQs) at the very low ng mL(-1) level, covering the range of expected concentrations for target compounds in red and white wines. For 38 out of 39 compounds, performance of sample preparation and determination steps were hardly affected by the wine matrix; thus, accurate recoveries were achieved by using pseudo-external calibration. Levels of target compounds in a set of 25 wine samples are reported. The capabilities of the described approach for the post-run identification of species not considered during method development, without retention time information, are illustrated and discussed with selected examples of compounds from different classes. PMID:26971021

  8. Automated storage of gas chromatography-mass spectrometry data in a relational database to facilitate compound screening and identification.

    Science.gov (United States)

    Staeb, J A; Epema, O J; van Duijn, P; Steevens, J; Klap, V A; Freriks, I L

    2002-10-18

    This paper describes a database containing massspectra from gas chromatography-mass spectrometry(GC-MS) measurements as a tool for easy screening for multiple compounds. In this way additional compounds can be reported from the same run together with routine pesticide monitoring with little effort. The relevant analytical data from the GC-MS measurements are transferred automatically to a database. Search algorithms in the database, containing the US EPA and Dutch NEN GC-MS identification criteria as standard settings, are used to identify compounds in the data. Screening of samples analysed in our laboratory show the ubiquitous presence of--up until now in monitoring largely overlooked--compounds in surface waters in The Netherlands. Most frequently found compounds include TAED (complexing agent), 2-methyl quinoline (industrial solvent), atrazin and desethylatrazin (pesticide and degradation product), caffeine (human consumption), surfinol-104 (anti foaming agent), HHCB (Galaxolide) and AHTN (Tonalide; fragrances). The database can also be used to quickly search a large number of datafiles for rare contaminants. This way, some interesting compounds such as pentoxifilin (a pharmaceutical) and Irgarol 1051 (an antifouling compound) were found. PMID:12458939

  9. Determination of free amino compounds in betalainic fruits and vegetables by gas chromatography with flame ionization and mass spectrometric detection.

    Science.gov (United States)

    Kugler, Florian; Graneis, Stephan; Schreiter, Pat P-Y; Stintzing, Florian C; Carle, Reinhold

    2006-06-14

    Amino acids and amines are the precursors of betalains. Therefore, the profiles of free amino compounds in juices obtained from cactus pears [Opuntia ficus-indica (L.) Mill. cv. Bianca, cv. Gialla, and cv. Rossa], pitaya fruits [Selenicereus megalanthus (K. Schumann ex Vaupel) Moran, Hylocereus polyrhizus (Weber) Britton & Rose, and Hylocereus undatus (Haworth) Britton & Rose], and in extracts from differently colored Swiss chard [Beta vulgaris L. ssp. cicla (L.) Alef. cv. Bright Lights] petioles and red and yellow beets (B. vulgaris L. ssp. vulgaris var. conditiva Alef. cv. Burpee's Golden) were investigated for the first time. Amino compounds were derivatized with propyl chloroformate. While gas chromatography (GC) with mass spectrometry was used for peak assignment, GC flame ionization detection was applied for quantification of individual compounds. Whereas proline was the major free amino compound of cactus pear and pitaya fruit juices, glutamine dominated in Swiss chard stems and beets, respectively. Interestingly, extremely high concentrations of dopamine were detected in Swiss chard stems and beets. Furthermore, the cleavage of betaxanthins caused by derivatization in alkaline reaction solutions is demonstrated for the first time. Amino acids and amines thus released might increase the actual free amino compound contents of the respective sample. To evaluate the contribution of betaxanthin cleavage to total amino acid and amine concentration, isolated betaxanthins were derivatized according to the "EZ:faast" method prior to quantification of the respective amino compounds released. On a molar basis, betaxanthin contribution to overall amino compound contents was always below 6.4%. PMID:16756361

  10. Analysis of organochlorine compounds in effluents from bleacheries by neutron activation analysis and gas chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Effluents from chlorine bleacheries in a sulfite and a sulfate paper plant have been investigated. The total amounts of nonpolar and phenolic organohalogenated compounds have been determined by neutron activation analysis. In the sulfate plant nonpolar (cyclohexane extractable) and phenolic (butyl acetate extractable) chlorinated compounds are present in concentrations of 0.36 and 1.7 ppm, respectively. In the sulfite plant both chlorinated and brominated compounds are present in average concentrations of 0.67 ppm Cl and 0.06 ppm Br for nonpolar compounds and 1.1 ppm Cl and 0.1 ppm Br for phenolic compounds. The occurrence of organobromine compounds in the sulfite plant is due to the use of seawater in the first chlorination step. The effluents have also been analysed by gas chromatography/mass spectrometry, and a number of halogenated aromatic hydrocarbons have been identified. These include chloro-p-methylisopropylbenzene (2 isomers), dichloro-p-methylisopropylbenzene (2 isomers), bromo-p-methylisopropylbenzene, chloro-p-methylisopropenylbenzene (2 isomers) and dichloro-p-methylisopropenylbenzene (2 isomers). These compounds are presumably formed by substitution reactions of the parent molecules which are formed by the cooking of the terpenes naturally present in wood. (author)

  11. Intercomparison of inductively coupled plasma mass spectrometry, quantitative neutron capture radiography, and prompt gamma activation analysis for the determination of boron in biological samples.

    Science.gov (United States)

    Schütz, C L; Brochhausen, C; Hampel, G; Iffland, D; Kuczewski, B; Otto, G; Schmitz, T; Stieghorst, C; Kratz, J V

    2012-10-01

    Boron determination in blood and tissue samples is a crucial task especially for treatment planning, preclinical research, and clinical application of boron neutron capture therapy (BNCT). Comparison of clinical findings remains difficult due to a variety of analytical methods, protocols, and standard reference materials in use. This paper addresses the comparability of inductively coupled plasma mass spectrometry, quantitative neutron capture radiography, and prompt gamma activation analysis for the determination of boron in biological samples. It was possible to demonstrate that three different methods relying on three different principles of sample preparation and boron detection can be validated against each other and yield consistent results for both blood and tissue samples. The samples were obtained during a clinical study for the application of BNCT for liver malignancies and therefore represent a realistic situation for boron analysis. PMID:22918535

  12. Intercomparison of inductively coupled plasma mass spectrometry, quantitative neutron capture radiography, and prompt gamma activation analysis for the determination of boron in biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Schuetz, C.L. [University of Mainz, Institute for Nuclear Chemistry, Mainz (Germany); Johannes Gutenberg-University of Mainz, Institute for Nuclear Chemistry, Mainz (Germany); Brochhausen, C. [University of Mainz, Institute of Pathology, Mainz (Germany); Hampel, G.; Iffland, D.; Schmitz, T.; Stieghorst, C.; Kratz, J.V. [University of Mainz, Institute for Nuclear Chemistry, Mainz (Germany); Kuczewski, B. [Regional Council Darmstadt, Darmstadt (Germany); Otto, G. [University of Mainz, Department of Hepatobiliary, Pancreatic and Transplantation Surgery, Mainz (Germany)

    2012-10-15

    Boron determination in blood and tissue samples is a crucial task especially for treatment planning, preclinical research, and clinical application of boron neutron capture therapy (BNCT). Comparison of clinical findings remains difficult due to a variety of analytical methods, protocols, and standard reference materials in use. This paper addresses the comparability of inductively coupled plasma mass spectrometry, quantitative neutron capture radiography, and prompt gamma activation analysis for the determination of boron in biological samples. It was possible to demonstrate that three different methods relying on three different principles of sample preparation and boron detection can be validated against each other and yield consistent results for both blood and tissue samples. The samples were obtained during a clinical study for the application of BNCT for liver malignancies and therefore represent a realistic situation for boron analysis. (orig.)

  13. Intercomparison of inductively coupled plasma mass spectrometry, quantitative neutron capture radiography, and prompt gamma activation analysis for the determination of boron in biological samples

    International Nuclear Information System (INIS)

    Boron determination in blood and tissue samples is a crucial task especially for treatment planning, preclinical research, and clinical application of boron neutron capture therapy (BNCT). Comparison of clinical findings remains difficult due to a variety of analytical methods, protocols, and standard reference materials in use. This paper addresses the comparability of inductively coupled plasma mass spectrometry, quantitative neutron capture radiography, and prompt gamma activation analysis for the determination of boron in biological samples. It was possible to demonstrate that three different methods relying on three different principles of sample preparation and boron detection can be validated against each other and yield consistent results for both blood and tissue samples. The samples were obtained during a clinical study for the application of BNCT for liver malignancies and therefore represent a realistic situation for boron analysis. (orig.)

  14. Analysis of triptophenolide and its related compounds from Tripterygium wilfordii Hook.f by electrospray ionization tandem mass spectrometry

    Science.gov (United States)

    Li, Rui; Peng, Aihua; He, Chunmei; Wang, Xianhuo; Shi, Jianyou; Chen, Lijuan; Wei, Yuquan

    2008-11-01

    Triptophenolide and its related compounds from Tripterygium wilfordii Hook.f is a kind of diterpenoids which shows anti-inflammatory activity. To study the metabolites of triptophenolide related compounds, the fragmentation mechanisms of them were investigated by using negative electrospray tandem mass spectrometry. With the aid of high resolution of ESI-QTOF-MS/MS, the fragmentation mechanisms of six diterpenoid compounds were systematically investigated. The fragmentation behavior mainly depends on what substituent groups the benzyl C ring bears. If there is a hydroxyl group on the position of C14, loss of CH4 is dominating. However, the successive loss of two CH3 radicals is predominant when the hydroxyl group of O14 is methylated. The lactone ring is prone to be dissociated to loss of CO, CO2 and C2H2O2 molecules. The pericyclic reaction can occur on A ring if there is an active hydrogen resides on C ring. Furthermore, one metabolite of compound A1 was confirmed by cytochrome P450 in vitro and the structure was proposed by tandem mass experiment together with the fragmentation mechanisms of this type of compounds.

  15. Elemental ratio measurements of organic compounds using aerosol mass spectrometry: characterization, improved calibration, and implications

    Directory of Open Access Journals (Sweden)

    M. R. Canagaratna

    2014-07-01

    Full Text Available Elemental compositions of organic aerosol (OA particles provide useful constraints on OA sources, chemical evolution, and effects. The Aerodyne high-resolution time-of-flight aerosol mass spectrometer (HR-ToF-AMS is widely used to measure OA elemental composition. This study evaluates AMS measurements of atomic oxygen-to-carbon (O : C, hydrogen-to-carbon (H : C, organic mass-to-organic carbon (OM : OC, and carbon oxidation state (OSC for a vastly expanded laboratory dataset of multifunctional oxidized OA standards. For the expanded standard dataset, the "Aiken-Explicit" method (Aiken et al., 2008, which uses experimentally measured ion intensities at all ions to determine elemental ratios, reproduces known molecular O : C and H : C ratio values within 20% (average absolute value of relative errors and 12% respectively. The more commonly used "Aiken-Ambient" method, which uses empirically estimated H2O+ and CO+ ion intensities to avoid gas phase air interferences at these ions, reproduces O : C and H : C of multifunctional oxidized species within 28% and 14% of known values. These values are systematically biased low, however, with larger biases observed for alcohols and simple diacids. A detailed examination of the H2O+, CO+, and CO2+ fragments in the high-resolution mass spectra of the standard compounds indicates that the Aiken-Ambient method underestimates the CO+ and H2O+ produced from many oxidized species. Combined AMS-vacuum ultraviolet (VUV ionization measurements indicate that these ions are produced by dehydration and decarboxylation on the AMS vaporizer (usually operated at 600 °C. Thermal decomposition is observed to be efficient at vaporizer temperatures down to 200 °C. These results are used together to develop an "Improved-Ambient" elemental analysis method for AMS spectra measured in air. The Improved-Ambient method reduces the systematic biases and reproduces O : C (H : C ratios of individual oxidized standards within 28% (13

  16. Second-class currents and the muon neutrino rest mass in the muon capture processes by 6Li and 3He nuclei

    International Nuclear Information System (INIS)

    The influence of second class currents (SCC) and that of the muon neutrino rest mass (mνμ) on the differential muon capture rate by the 6Li and 3He, and on the angular asymmetry coefficient (aμν) of the neutrino emission direction with respect to the muon spin orientation, is investigated. It is shown that the experimental study of aμν may give an efficient estimation for mνμ and for SCC form factors FT (in the case of 6Li and 3He) and FS (in the case of 3He). 26 refs

  17. COMPARISON OF TIME-OF-FLIGHT AND DOUBLE FOCUSING MASS SPECTROMETRY FOR REACHING TENTATIVE IDENTIFICATIONS FOR UNANTICIPATED COMPOUNDS ADDED TO DRINKING WATER BY TERRORISTS

    Science.gov (United States)

    Local monitoring of post-treatment drinking water using bench-top mass spectrometers could identify target compounds in a mass spectral library. However, a terrorist might seek to incite greater hysteria by injecting or infusing a mixture of unanticipated compounds of unknown tox...

  18. Mass transfer coeficient for the prediction of volatile organic compound evaporation rate from water basin : Effect of wind speed

    OpenAIRE

    Bunyakan, C.; Tongsoy, P.; Tongurai, C.

    2001-01-01

    Recently, volatile organic compound (VOC) evaporation from open water basin such as an equalization basin in wasterwater treatment plant has been recognized as an important source of air polution. The amount of VOC evaporation from open water basin can be predicted by using the two-film theory that requires two mass transfer coefficients includint kG and kL. This paper studies the effect of wind speed over sater surface on the gas-film (kG) and the liquid-film (kL) mass transfer coefficient. ...

  19. A New Method to Diagnose Cancer Based on Image Analysis of Mass Chromatograms of Volatile Organic Compounds in Urine

    Directory of Open Access Journals (Sweden)

    Rozhentsov А.А.

    2014-12-01

    Full Text Available The aim of investigation was to develop a technique to diagnose early cancer based on the image analysis of mass chromatograms of volatile organic compounds in urine, and assess its efficacy. Materials and Methods. The patients were grouped by nosological types: lung cancer, esophageal cancer, gastric carcinoma, colon cancer. A control group consisted of healthy individuals. Metabolic profiles of volatile organic compounds of urine were obtained using head space solid phase microextraction coupled to gas chromatography — mass spectrometry method. Results. In accordance with the processed data of mass chromatograms of volatile organic compounds of urine for each patient and their comparison with images of control individuals, we made reference metabolic profiles of oncological diseases. The proposed technique for cancer detection is easy, non-invasive, low labor intensive and affordable. According to the assessment of the results obtained, the method sensitivity is 100%, specificity — 90.62%, type I error probability — 0%, type II error probability — 9.38%. Conclusion. The findings could be used for the further understanding of etiology and pathology of various forms of oncological diseases.

  20. Precision Mass Measurements of ^{129-131}Cd and Their Impact on Stellar Nucleosynthesis via the Rapid Neutron Capture Process.

    Science.gov (United States)

    Atanasov, D; Ascher, P; Blaum, K; Cakirli, R B; Cocolios, T E; George, S; Goriely, S; Herfurth, F; Janka, H-T; Just, O; Kowalska, M; Kreim, S; Kisler, D; Litvinov, Yu A; Lunney, D; Manea, V; Neidherr, D; Rosenbusch, M; Schweikhard, L; Welker, A; Wienholtz, F; Wolf, R N; Zuber, K

    2015-12-01

    Masses adjacent to the classical waiting-point nuclide ^{130}Cd have been measured by using the Penning-trap spectrometer ISOLTRAP at ISOLDE/CERN. We find a significant deviation of over 400 keV from earlier values evaluated by using nuclear beta-decay data. The new measurements show the reduction of the N=82 shell gap below the doubly magic ^{132}Sn. The nucleosynthesis associated with the ejected wind from type-II supernovae as well as from compact object binary mergers is studied, by using state-of-the-art hydrodynamic simulations. We find a consistent and direct impact of the newly measured masses on the calculated abundances in the A=128-132 region and a reduction of the uncertainties from the precision mass input data. PMID:26684113

  1. HOLMES - The Electron Capture Decay of 163Ho to Measure the Electron Neutrino Mass with sub-eV sensitivity

    CERN Document Server

    Alpert, B; Bennett, D; Biasotti, M; Boragno, C; Brofferio, C; Ceriale, V; Corsini, D; De Gerone, M; Dressler, R; Faverzani, M; Ferri, E; Fowler, J; Gatti, F; Giachero, A; Hays-Wehle, J; Heinitz, S; Hilton, G; Koester, U; Lusignoli, M; Maino, M; Mates, J; Nisi, S; Nizzolo, R; Nucciotti, A; Pessina, G; Pizzigoni, G; Puiu, A; Ragazzi, S; Reintsema, C; Gomes, M Ribeiro; Schmidt, D; Schumann, D; Sisti, M; Swetz, D; Terranova, F; Ullom, J

    2014-01-01

    The European Research Council has recently funded HOLMES, a new experiment to directly measure the neutrino mass. HOLMES will perform a calorimetric measurement of the energy released in the decay of 163Ho. The calorimetric measurement eliminates systematic uncertainties arising from the use of external beta sources, as in experiments with beta spectrometers. This measurement was proposed in 1982 by A. De Rujula and M. Lusignoli, but only recently the detector technological progress allowed to design a sensitive experiment. HOLMES will deploy a large array of low temperature microcalorimeters with implanted 163Ho nuclei. The resulting mass sensitivity will be as low as 0.4 eV. HOLMES will be an important step forward in the direct neutrino mass measurement with a calorimetric approach as an alternative to spectrometry. It will also establish the potential of this approach to extend the sensitivity down to 0.1 eV. We outline here the project with its technical challenges and perspectives.

  2. Precision Mass Measurements of 129-131Cd and Their Impact on Stellar Nucleosynthesis via the Rapid Neutron Capture Process

    CERN Document Server

    Atanasov, D; Blaum, K; Cakirli, R B; Cocolios, T E; George, S; Herfurth, F; Kisler, D; Kowalska, M; Kreim, S; Litvinov, Yu A; Lunney, D; Manea, V; Neidherr, D; Rosenbusch, M; Schweikhard, L; Welker, A; Wienholtz, F; Wolf, R N; Zuber, K

    2015-01-01

    Masses adjacent to the classical waiting-point nuclide 130Cd have been measured by using the Penning- trap spectrometer ISOLTRAP at ISOLDE/CERN. We find a significant deviation of over 400 keV from earlier values evaluated by using nuclear beta-decay data. The new measurements show the reduction of the N = 82 shell gap below the doubly magic 132Sn. The nucleosynthesis associated with the ejected wind from type-II supernovae as well as from compact object binary mergers is studied, by using state-of-the-art hydrodynamic simulations. We find a consistent and direct impact of the newly measured masses on the calculated abundances in the A = 128 - 132 region and a reduction of the uncertainties from the precision mass input data.

  3. Disjunct eddy covariance measurements of volatile organic compound fluxes using proton transfer reaction mass spectrometry

    OpenAIRE

    Taipale, Risto

    2011-01-01

    Volatile organic compounds (VOCs) are emitted into the atmosphere from natural and anthropogenic sources, vegetation being the dominant source on a global scale. Some of these reactive compounds are deemed major contributors or inhibitors to aerosol particle formation and growth, thus making VOC measurements essential for current climate change research. This thesis discusses ecosystem scale VOC fluxes measured above a boreal Scots pine dominated forest in southern Finland. The flux measureme...

  4. Analysis of Volatile Compounds of Malaysian Tualang (Koompassia Excelsa) Honey Using Gas Chromatography Mass Spectrometry

    OpenAIRE

    Nurul Syazana, MS; Gan, SH; Halim, AS; Shah, Nurul Syazana Mohamad; Gan, Siew Hua; Sukari, Halim Ahmad

    2012-01-01

    The constituents of honey's volatile compounds depend on the nectar source and differ depending on the place of origin. To date, the volatile constituents of Tualang honey have never been investigated. The objective of this study was to analyze the volatile compounds in local Malaysian Tualang honey. A continuous extraction of Tualang honey using five organic solvents was carried out starting from non-polar to polar solvents and the extracted samples were analysed using gas chromatography-mas...

  5. Determination of the neutrino mass by electron capture in 163 Holmium and the role of the three-hole states in 163 Dysprosium

    CERN Document Server

    Faessler, Amand; Gastaldo, Loredana; Simkovic, F

    2015-01-01

    163 Holmium to 163 Dysprosium is probably due to the small Q value of about 2.5 keV the best case to determine the neutrino mass by electron capture. The energy of the Q value is distributed between the excitation of Dysprosium (and the neglected small recoil of Holmium) and the relativistic energy of the emitted neutrino including the restmass. The reduction of the upper end of the deexcitation spectrum of Dysprosium below the Q value allows to determine the neutrino mass. The excitation of Dysprosium can be calculated in the sudden approximation of the overlap of the electron wave functions of Holmium minus the captured electron and one-, two-, three- and multiple hole-excitations in Dysprosium. Robertson and the author have calculated the influence of the two-hole states on the Dysprosium deexitation spectrum. Here for the first time the influence of the three-hole states on the deexcitation bolometer spectrum of 163 Dysprosium is presented. The electron wave functions and the overlaps are calculated selfc...

  6. Neutrinoless double electron capture

    CERN Document Server

    Kotila, J; Iachello, F

    2015-01-01

    Direct determination of the neutrino mass is at the present time one of the most important aims of experimental and theoretical research in nuclear and particle physics. A possible way of detection is through neutrinoless double electron capture, $0\

  7. Analysis of volatile compounds responsible for kiwifruit aroma by desiccated headspace gas chromatography-mass spectrometry.

    Science.gov (United States)

    Zhang, Chun-Yun; Zhang, Qiong; Zhong, Cai-Hong; Guo, Ming-Quan

    2016-04-01

    A new method for desiccated headspace (DHS) sampling of aqueous sample to GC-MS for the analysis of volatile compounds responsible for kiwifruit aroma in different kiwifruit cultivars has been developed based on the complete hydrate formation between the sample solvent (water) with anhydrous salt (calcium chloride) at an elevated temperature (above the boiling point of the aqueous sample) in a non-contact format, which overcame the water-effect challenge to directly introduce aqueous sample into GC-MS analysis. By means of DHS, the volatile compounds in three different kiwifruit cultivars were analyzed and compared under the optimized operating conditions, mainly time and temperature for headspace equilibration, column temperature program for GC-MS measurement. As a result, 20 peaks of volatile compounds responsible for kiwifruit aroma were detected and remarkable differences were found in the relative contents of three major volatile compounds among the three different kiwifruit cultivars, i.e., acetaldehyde, ethanol and furfural. The DHS sampling technique used in the present method can make the GC-MS analysis of volatile compounds in the aqueous sample within complex matrix possible without contaminating the GC-MS instrument. In terms of the analysis of volatile compounds in kiwifruit, the present method enabled a direct measurement on the filtrate of the aqueous kiwifruit pulp, without intermediate trap phase for the extraction of analytes, which will be more reliable and simpler as compared with any other headspace method in use. Thus, DHS coupled with GC-MS will be a new valuable tool available for the kiwifruit related research and organoleptic quality control. PMID:26922094

  8. Laser desorption and matrix-assisted laser desorption/ionization mass spectrometry of 29-kDa Au:SR cluster compounds.

    Science.gov (United States)

    Schaaff, T Gregory

    2004-11-01

    Positive and negative ions generated by laser-based ionization methods from three gold:thiolate cluster compounds are mass analyzed by time-of-flight mass spectrometry. The three compounds have similar inorganic core masses ( approximately 29 kDa, approximately 145 Au atoms) but different n-alkanethiolate ligands associated with each cluster compound (Au:SR, R = butane, hexane, dodecane). Irradiation of neat films (laser desorption/ionization) and films generated by dilution of the cluster compounds in an organic acid matrix (matrix-assisted laser desorption/ionization) with a nitrogen laser (337 nm) produced distinct ion abundances that are relevant to different structural aspects of the cluster compound. Laser desorption/ionization of neat Au:SR compound films produces ions consistent with the inorganic core mass (i.e., devoid of original hydrocarbon content). Matrix-assisted laser desorption/ionization produces either ions with m/z values consistent with the core mass of the cluster compounds or ions with m/z values consistent with the approximate molecular weight of the cluster compounds, depending on ionization conditions. The ion abundances, and ionization conditions under which they are detected, provide insight into desorption/ionization processes for these unique cluster compounds as well as other analytes typically studied by matrix-assisted laser desorption/ionization. PMID:15516109

  9. ANALYSIS OF CHEMICAL COMPOUNDS OF AGARWOOD OIL FROM DIFFERENT SPECIES BY GAS CHROMATOGRAPHY MASS SPECTROMETRY (GCMS)

    OpenAIRE

    Yumi Zuhanis Has-Yun Hashim; Nur Izzah Ismail; Phirdaous Abbas

    2014-01-01

    ABSTRACT: Agarwood oil is a highly prized type of oil due to its unique aroma. The oil is extracted from the fragrant resin found in the agarwood tree (trunk).  The unique aroma and quality of agarwood resin and oil are contributed by the presence of certain chemical compounds. In this work, analysis and comparison of the chemical compounds of agarwood oil from A. malaccensis, A. sub-integra and a mixture of both were conducted.  The essential oils were diluted in hexane (5%) prior to gas chr...

  10. Cure of malignant melanoma by single thermal neutron capture treatment using melanoma-seeking compounds: 10B/melanogenesis interaction to in vitro/in vivo radiobiological analysis to preclinical studies

    International Nuclear Information System (INIS)

    This paper discusses the synthesis of new tumor-seeking 10B-compounds which possess selective affinity for the specific metabolic activity of the target cancer cells. Since not only malignant melanomas but also many kinds of human cancers, for example thyroid cancer and squamous cell carcinoma, synthesize their specific protein, the aim is to establish selective thermal neutron capture treatment of malignant melanoma as a prototype of such cancer cells

  11. Analysis of volatile organic compounds using proton-transfer-reaction-mass spectrometry (PTR-MS) in the ppb range

    International Nuclear Information System (INIS)

    Gas-Chromatographic methods have been used most successfully to analyze quantitatively the concentrations of VOC's relevant to environmental as well as medical applications. Gas samples that have been collected by cryogenic methods or by absorption techniques are separated on a GC-column and then analyzed by a mass spectrometer. Pre-concentrating and drying are necessary steps in this kind of analysis and might be significant sources of loosing quantitative concentrations of VOC's. Mass spectrometric methods are usually less sensitive but have the advantage of being extremely fast, so that on-fine measurements can be done. However, when electron impact or charge transfer processes are used to ionize the compounds of interest the resulting molecular ions show strong fragmentation. Identification and quantitative correlation of specific compounds in mixtures of VOC's is complicated, because fragmentation patterns of several compounds often show strong overlap. Fragmentation can be completely avoided for many VOC's, when ionization occurs via proton transfer from the proton-donor H3O+

  12. In vivo analysis of palm wine (Elaeis guineensis) volatile organic compounds (VOCs) by proton transfer reaction-mass spectrometry

    Science.gov (United States)

    Lasekan, Ola; Otto, Sabine

    2009-04-01

    The in vivo volatile organic compounds (VOCs) release patterns in palm wine was carried out using the PTR-MS. In order to analyze the complex mixtures of VOCs in palm wine, the fragmentation patterns of 14 known aroma compounds of palm wine were also investigated. Results revealed masses m/z (43, 47, 61, 65, 75, 89 and 93) as the predominant ones measured in-breathe exhaled from the nose, during consumption of palm wine. Further studies of aroma's fragmentation patterns, showed that the m/z 43 is characteristic of fragment of various compounds, while m/z 47 is ethanol, m/z 61(acetic acid), m/z 65 (protonated ethanol cluster ions), m/z 75 (methyl acetate), m/z 89 (acetoin) and m/z 93 (2-phenylethanol) respectively. The dynamic release parameters (Imax and tmax) of the 7 masses revealed significant (P = 0.05) differences, between maximum intensity (Imax) and no significant (P = 0.05) differences between tmax among VOCs respectively.

  13. Studies on effective atomic numbers, electron densities from mass attenuation coefficients near the K edge in some samarium compounds

    International Nuclear Information System (INIS)

    The effective atomic numbers and electron densities of some samarium compounds were determined using the experimental total mass attenuation coefficient values near the K edge in the X-ray energy range from 36.847 up to 57.142 keV. The measurements, in the region from 36.847 to 57.142 keV, were done in a transmission geometry utilizing the Kα2, Kα1, Kβ1 and Kβ2 X-rays from different secondary source targets excited by the 59.54 keV gamma-photons from an Am-241 annular source. This paper presents the first measurement of the effective atomic numbers and electron densities for some samarium compounds near the K edge. The results of the study showed that the measured values were in good agreement with the theoretically calculated ones. - Highlights: • The effective atomic numbers and electron densities determined for some samarium compounds from total mass attenuation coefficients near the K edge. • The measurements performed using secondary excitation geometry and a Si(Li) detector. • The experimental results compared with the theoretical calculation

  14. Identification of phenolic compounds in strawberries by liquid chromatography electrospray ionization mass spectroscopy

    OpenAIRE

    Seeram, Navindra P.; Lee, R; Scheuller, H S; Heber, D

    2006-01-01

    Strawberry (Fragaria x ananassa Duch.) fruits contain phenolic compounds that have antioxidant, anticancer, antiatherosclerotic and anti-neurodegenerative properties. Identification of food phenolics is necessary since their nature, size, solubility, degree and position of glycosylation and conjugation influence their absorption, distribution, metabolism and excretion in humans. Freeze-dried whole strawberry fruit powder and strawberry fruit extracts were analyzed by liquid chromatography ele...

  15. Comprehensive Analysis of Umami Compounds by Ion-Pair Liquid Chromatography Coupled to Mass Spectrometry

    NARCIS (Netherlands)

    Coulier, L.; Bas, R.; Hekman, M.; Werff, B.J.C. van der; Burgering, M.; Thissen, U.

    2011-01-01

    An ion-pair LC-ESI-MS method was developed capable of analyzing various reported umami or umami-enhancing compounds, including glutamic acid and 5'-ribonucleotides. The method was validated using tomato and potato samples and showed overall good analytical performance with respect to selectivity, de

  16. Tidal capture formation of low-mass X-ray binaries from wide binaries in the field

    Science.gov (United States)

    Michaely, Erez; Perets, Hagai B.

    2016-06-01

    We present a dynamical formation scenario for low mass X-ray binaries (LMXBs) in the field, focusing on black hole (BH) LMXBs. In this formation channel, LMXBs are formed from wide binaries (>1000 au) with a BH component and a stellar companion. The wide binary is perturbed by fly-bys of field stars, its orbit random walks, until driven into a sufficiently eccentric orbit such that the binary components tidally interact and the binary evolves to become a short period binary, which eventually evolves into an LMXB. We consider several models for the formation and survival of such wide binaries, and calculate the LMXB formation rates for each model. We find that models where BHs form through direct collapse with no/little natal kicks can give rise to high formation rates comparable with those inferred from observations. This formation scenario had several observational signatures: (1) the number density of LMXBs generally follows the background stellar density, beside the densest regions, where the dependence is stronger, (2) the mass function of the BH stellar companion should be comparable to the mass function of the background stellar population, likely peaking at 0.4-0.6 M⊙, and (3) the LMXBs orbit should not correlate with the spin of the BH. These aspects generally differ from the expectations from previously suggested LMXB formation models following common envelope binary stellar evolution. We note that neutron star LMXBs can similarly form from wide binaries, but their formation rate through this channel is likely significantly smaller due to their much higher natal kicks.

  17. Separation of 163Er from dysprosium target. A step toward neutrino mass measurement through electron capture of 163Ho

    International Nuclear Information System (INIS)

    Production of pure 163Ho, a potential source for the direct kinematic measurement of neutrino mass, via the decay of its precursor 163Er has been investigated. The short-lived 163Er (75 min) will be produced in the α-particle induced reaction on natural Dy oxide target and will decay eventually to 163Ho. A fast radiochemical separation technique based on liquid-liquid extraction using di-(2-ethylhexyl)phosphoric acid (HDEHP) dissolved in cyclohexane as organic phase and HCl as aqueous phase has been developed to separate no-carrier added (NCA) Er from the Dy matrix. (author)

  18. Mass spectrometric analysis of stable carbon isotopes in abiogenic and biogenic natural compounds

    International Nuclear Information System (INIS)

    This report describes the general methodology of sup/13/ carbon analysis on mass spectrometer and various preparation systems developed for conversion of samples into isotopically non-fractionated and purified carbon dioxide. Laboratory standards required for sup/13/ C analysis have been calibrated against international standards. The reproducibility/accuracy of sample preparation and analysis on mass spectrometer for sup/13/ C or sup/12/ C measurement is well within the internationally acceptable limits. (author)

  19. Influence of dissolved humic substances on the mass transfer of organic compounds across the air-water interface.

    Science.gov (United States)

    Ramus, Ksenia; Kopinke, Frank-Dieter; Georgi, Anett

    2012-01-01

    The effect of dissolved humic substances (DHS) on the rate of water-gas exchange of two volatile organic compounds was studied under various conditions of agitation intensity, solution pH and ionic strength. Mass-transfer coefficients were determined from the rate of depletion of model compounds from an apparatus containing a stirred aqueous solution with continuous purging of the headspace above the solution (dynamic system). Under these conditions, the overall transfer rate is controlled by the mass-transfer resistance on the water side of the water-gas interface. The experimental results show that the presence of DHS hinders the transport of the organic molecules from the water into the gas phase under all investigated conditions. Mass-transfer coefficients were significantly reduced even by low, environmentally relevant concentrations of DHS. The retardation effect increased with increasing DHS concentration. The magnitude of the retardation effect on water-gas exchange was compared for Suwannee River fulvic and humic acids, a commercially available leonardite humic acid and two synthetic surfactants. The observed results are in accordance with the concept of hydrodynamic effects. Surface pressure forces due to surface film formation change the hydrodynamic characteristics of water motion at the water-air interface and thus impede surface renewal. PMID:22051345

  20. Improved Description of One- and Two-Hole States after Electron Capture in 163 Holmium and the Determination of the Neutrino Mass

    CERN Document Server

    Faessler, Amand

    2015-01-01

    The atomic pair 163 Holmium and 163 Dysprosium$ seems due to the small Q value of about 2.3 to 2.8 keV the best case to determine the neutrino mass by electron capture. The bolometer spectrum measures the full deexcitation energy of Dysprosium by X rays, by Auger electrons and by the recoil of Holmium. The spectrum has an upper energy limit given by the Q value minus the neutrino mass. Till now this spectrum has been calculated allowing in Dysprosium excitations with 3s1/2, 3p1/2, 4s1/2, 4p1/2, 5s1/2, 5p1/2 holes only. Robertson calculated recently also the spectrum with two electron hole excitations in Dy. He took the probability for the excitation for the second electron hole from work of Carlson and Nestor for Z=54 Xenon. He claims, that the bolometer spectrum with two holes is "not well enough understood to permit a sensitive determination of the neutrino mass in this way." The purpose of the present work is to determine the theoretical bolometer spectrum with two hole excitations more reliably. In additi...

  1. Specific interaction between negative atmospheric ions and organic compounds in atmospheric pressure corona discharge ionization mass spectrometry.

    Science.gov (United States)

    Sekimoto, Kanako; Sakai, Mami; Takayama, Mitsuo

    2012-06-01

    The interaction between negative atmospheric ions and various types of organic compounds were investigated using atmospheric pressure corona discharge ionization (APCDI) mass spectrometry. Atmospheric negative ions such as O(2)(-), HCO(3)(-), COO(-)(COOH), NO(2)(-), NO(3)(-), and NO(3)(-)(HNO(3)) having different proton affinities served as the reactant ions for analyte ionization in APCDI in negative-ion mode. The individual atmospheric ions specifically ionized aliphatic and aromatic compounds with various functional groups as atmospheric ion adducts and deprotonated analytes. The formation of the atmospheric ion adducts under certain discharge conditions is most likely attributable to the affinity between the analyte and atmospheric ion and the concentration of the atmospheric ion produced under these conditions. The deprotonated analytes, in contrast, were generated from the adducts of the atmospheric ions with higher proton affinity attributable to efficient proton abstraction from the analyte by the atmospheric ion. PMID:22528201

  2. Studies on effective atomic numbers, electron densities from mass attenuation coefficients near the K edge in some samarium compounds.

    Science.gov (United States)

    Akman, F; Durak, R; Turhan, M F; Kaçal, M R

    2015-07-01

    The effective atomic numbers and electron densities of some samarium compounds were determined using the experimental total mass attenuation coefficient values near the K edge in the X-ray energy range from 36.847 up to 57.142 keV. The measurements, in the region from 36.847 to 57.142 keV, were done in a transmission geometry utilizing the Kα2, Kα1, Kβ1 and Kβ2 X-rays from different secondary source targets excited by the 59.54 keV gamma-photons from an Am-241 annular source. This paper presents the first measurement of the effective atomic numbers and electron densities for some samarium compounds near the K edge. The results of the study showed that the measured values were in good agreement with the theoretically calculated ones. PMID:25880612

  3. Boron neutron capture therapy of brain tumors: investigation of urinary metabolites and oxidation products of sodium borocaptate by electrospray ionization mass spectrometry.

    Science.gov (United States)

    Gibson, C R; Staubus, A E; Barth, R F; Yang, W; Kleinholz, N M; Jones, R B; Green-Church, K; Tjarks, W; Soloway, A H

    2001-12-01

    Boron neutron capture therapy (BNCT) is based on a nuclear capture reaction that occurs when boron-10, a stable isotope, is irradiated with low energy neutrons to produce high-energy alpha particles and recoiling lithium-7 nuclei. The purpose of the present study was to determine what urinary metabolites, if any, could be detected in patients with brain tumors who were given sodium borocaptate (BSH), a drug that has been used clinically for BNCT. BSH was infused intravenously over a 1-h time period at doses of 26.5, 44.1, or 88.2 mg/kg of body weight to patients with high-grade brain tumors. Electrospray ionization mass spectrometry has been used to investigate possible urinary metabolites of BSH. Chemical and instrument conditions were established to detect BSH and its possible metabolites in both positive and negative electrospray ionization modes. Using this methodology, boronated ions were found in patients' urine samples that appeared to be consistent with the following chemical structures: BSH sulfenic acid (BSOH), BSH sulfinic acid (BSO(2)H), BSH disulfide (BSSB), BSH thiosulfinate (BSOSB), and a BSH-S-cysteine conjugate (BSH-CYS). Although BSH has been used clinically for BNCT since the late 1960s, this is the first report of specific biotransformation products following administration to patients. Further studies will be required to determine both the biological significance of these metabolites and whether any of these accumulate in significant amounts in brain tumors. PMID:11717178

  4. Matrix-assisted laser desorption fourier transform mass spectrometry for biological compounds

    Energy Technology Data Exchange (ETDEWEB)

    Hettich, R.; Buchanan, M.

    1990-01-01

    The recent development of matrix-assisted UV laser desorption (LD) mass spectrometry has made possible the ionization and detection of extremely large molecules (with molecular weights exceeding 100,000 Daltons). This technique has generated enormous interest in the biological community for the direct examination of large peptides and oligonucleotides. Although this matrix-assisted ionization method has been developed and used almost exclusively with time-of-flight (TOF) mass spectrometers, research is currently in progress to demonstrate this technique with trapped ion mass spectrometers, such as Fourier transform ion cyclotron resonance mass spectrometry (FTMS). The potential capabilities of FTMS for wide mass range, high resolution measurement, and ion trapping experiments suggest that this instrumental technique should be useful for the detailed structural characterization of large ions generated by the matrix-assisted technique. We have recently demonstrated that matrix-assisted ultraviolet laser desorption can be successfully used with FTMS for the ionization of small peptides. The objective of this report is to summarize the application and current limitations of matrix-assisted laser desorption FTMS for the characterization of peptides and oligonucleotides at the isomeric level. 4 refs., 3 figs., 2 tabs.

  5. MANTRA: An Integral Reactor Physics Experiment to Infer Actinide Capture Cross-sections from Thorium to Californium with Accelerator Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    G. Youinou; C. McGrath; G. Imel; M. Paul; R. Pardo; F. Kondev; M. Salvatores; G. Palmiotti

    2011-08-01

    The principle of the proposed experiment is to irradiate very pure actinide samples in the Advanced Test Reactor at INL and, after a given time, determine the amount of the different transmutation products. The determination of the nuclide densities before and after neutron irradiation will allow inference of effective neutron capture cross-sections. This approach has been used in the past and the novelty of this experiment is that the atom densities of the different transmutation products will be determined using the Accelerator Mass Spectrometry technique at the ATLAS facility located at ANL. It is currently planned to irradiate the following isotopes: 232Th, 235U, 236U, 238U, 237Np, 238Pu, 239Pu, 240Pu, 241Pu, 242Pu, 241Am, 243Am, 244Cm and 248Cm.

  6. Combined infrared multiphoton dissociation and electron-capture dissociation using co-linear and overlapping beams in Fourier transform ion cyclotron resonance mass spectrometry.

    Science.gov (United States)

    Mihalca, Romulus; van der Burgt, Yuri E M; McDonnell, Liam A; Duursma, Marc; Cerjak, Iliya; Heck, Albert J R; Heeren, Ron M A

    2006-01-01

    A novel set-up for Fourier transform ion cyclotron resonance mass spectrometry (FTICR) is reported for simultaneous infrared multiphoton dissociation (IRMPD) and electron-capture dissociation (ECD). An unmodified electron gun ensures complete, on-axis overlap between the electron and the photon beams. The instrumentation, design and implementation of this novel approach are described. In this configuration the IR beam is directed into the ICR cell using a pneumatically actuated mirror inserted into the ion-optical path. Concept validation was made using different combinations of IRMPD and ECD irradiation events on two standard peptides. The ability to perform efficient IRMPD, ECD and especially simultaneous IRMPD and ECD using lower irradiation times is demonstrated. The increase in primary sequence coverage, with the combined IRMPD and ECD set-up, also increases the confidence in peptide and protein assignments. PMID:16705647

  7. MANTRA: An Integral Reactor Physics Experiment to Infer Actinide Capture Cross-sections from Thorium to Californium with Accelerator Mass Spectrometry

    International Nuclear Information System (INIS)

    The principle of the proposed experiment is to irradiate very pure actinide samples in the Advanced Test Reactor at INL and, after a given time, determine the amount of the different transmutation products. The determination of the nuclide densities before and after neutron irradiation will allow inference of effective neutron capture cross-sections. This approach has been used in the past and the novelty of this experiment is that the atom densities of the different transmutation products will be determined using the Accelerator Mass Spectrometry technique at the ATLAS facility located at ANL. It is currently planned to irradiate the following isotopes: 232Th, 235U, 236U, 238U, 237Np, 238Pu, 239Pu, 240Pu, 241Pu, 242Pu, 241Am, 243Am, 244Cm and 248Cm.

  8. Methane mass balance at three landfill sites: What is the efficiency of capture by gas collection systems?

    International Nuclear Information System (INIS)

    Many developed countries have targeted landfill methane recovery among greenhouse gas mitigation strategies, since methane is the second most important greenhouse gas after carbon dioxide. Major questions remain with respect to actual methane production rates in field settings and the relative mass of methane that is recovered, emitted, oxidized by methanotrophic bacteria, laterally migrated, or temporarily stored within the landfill volume. This paper presents the results of extensive field campaigns at three landfill sites to elucidate the total methane balance and provide field measurements to quantify these pathways. We assessed the overall methane mass balance in field cells with a variety of designs, cover materials, and gas management strategies. Sites included different cell configurations, including temporary clay cover, final clay cover, geosynthetic clay liners, and geomembrane composite covers, and cells with and without gas collection systems. Methane emission rates ranged from -2.2 to >10,000 mg CH4 m-2 d-1. Total methane oxidation rates ranged from 4% to 50% of the methane flux through the cover at sites with positive emissions. Oxidation of atmospheric methane was occurring in vegetated soils above a geomembrane. The results of these studies were used as the basis for guidelines by the French environment agency (ADEME) for default values for percent recovery: 35% for an operating cell with an active landfill gas (LFG) recovery system, 65% for a temporary covered cell with an active LFG recovery system, 85% for a cell with clay final cover and active LFG recovery, and 90% for a cell with a geomembrane final cover and active LFG recovery

  9. Synthesis, Mass Spectrometric Studies, and Biological Evaluation of 3,5-Dimethoxyhomophthalic Acid and Related Compounds

    Institute of Scientific and Technical Information of China (English)

    GHULAM Qadeer; NASIM Hasan-rama; FAN Zhi-jin

    2007-01-01

    3,5-Dimethoxyhomophthalic acid was synthesized in four steps from 3,5-dimethoxycinnamic acid via a series of reactions including cyclization of 3-(3' ,5'-dimethoxyphenyl) propionic acid to 5,7-dimethoxy-1-indanone and oxidative decomposition of methyl-2-hydroxy-2-[ 5,7-dimethyoxy-1-oxo-1H-inden-2 (3H) -ylidene ] acetate to 3,5-dimethoxyhomophthalic acid. The synthesized compounds were characterized by elemental analysis, IR, 1H NMR, and MS. The biological evaluation experiments of 3,5-dimthoxyhomophthalic acid and the related synthesized compounds were also carried out. Naturally occurring biologically active isocoumarins were prepared in a single step by the condensation of the homophthalic acid with appropriate acid chlorides.

  10. Application of parallel liquid chromatography/mass spectrometry for high throughput microsomal stability screening of compound libraries.

    Science.gov (United States)

    Xu, Rongda; Nemes, Csaba; Jenkins, Kelly M; Rourick, Robyn A; Kassel, Daniel B; Liu, Charles Z C

    2002-02-01

    Solution-phase and solid-phase parallel synthesis and high throughput screening have enabled biologically active and selective compounds to be identified at an unprecedented rate. The challenge has been to convert these hits into viable development candidates. To accelerate the conversion of these hits into lead development candidates, early assessment of the physicochemical and pharmacological properties of these compounds is being made. In particular, in vitro absorption, distribution, metabolism, and elimination (ADME) assays are being conducted at earlier and earlier stages of discovery with the goal of reducing the attrition rate of these potential drug candidates as they progress through development. In this report, we present an eight-channel parallel liquid chromatography/mass spectrometry (LC/MS) system in combination with custom Visual Basic and Applescript automated data processing applications for high throughput early ADME. The parallel LC/MS system was configured with one set of gradient LC pumps and an eight-channel multiple probe autosampler. The flow was split equivalently into eight streams before the multiple probe autosampler and recombined after the eight columns and just prior to the mass spectrometer ion source. The system was tested for column-to-column variation and for reproducibility over a 17 h period (approximately 500 injections per column). The variations in retention time and peak area were determined to be less than 2 and 10%, respectively, in both tests. The parallel LC/MS system described permits time-course microsomal incubations (t(o), t5, t15, t30) to be measured in triplicate and enables estimations of t 1/2 microsomal stability. The parallel LC/MS system is capable of analyzing up to 240 samples per hour and permits the complete profiling up to two microtiter plates of compounds per day (i.e., 176 test substrate compounds + sixteen controls). PMID:11841071

  11. Analysis of carotenoid compounds in aphids by Raman imaging and mass spectrometry

    OpenAIRE

    sprotocols

    2015-01-01

    Authors: Pierre Brat, Jean Christophe Valmalette, Christian Mertz, George de Sousa, Aviv Dombrovsky, Maria Capovilla & Alain Robichon ### Abstract Carotenoids are compounds synthesized in plants, bacteria and fungi, closely associated to the chlorophyll to perform photosynthesis. A spectacular evolutionary achievement allowed the aphid to produce carotenoids obviously by lateral transfer of genes from fungi. We have recently documented that these molecules are involved in photo c...

  12. Mass spectrometric isomer characterization of perfluorinated compounds in technical mixture, water and human blood

    OpenAIRE

    Langlois, Ingrid

    2007-01-01

    Perfluorinated compounds (PFC) are special surfactants which have been used since the 1950s. Their detection in the environment started at the beginning of the 2000s. A lot has to be explored in different fields such as method development, understanding of their environmental distribution, human exposure and their transport to remote areas such as the Artic region. No degradation pathways are known for perfluorooctane sulfonate (PFOS) and perfluorooctanoic acid (PFOA), two pred...

  13. Direct thermal neutron capture

    International Nuclear Information System (INIS)

    We discuss the direct-capture theory pertaining to primary electric dipole (E1) transitions following slow-neutron capture. For light nuclides that we have studied (including 9Be, 12C, 13C, 24Mg, 25Mg, 26Mg, 32S, 33S, 34S, 40Ca, and 44Ca), estimates of direct-capture cross sections using optical-model potentials with physically realistic parameters, are in reasonable agreement with the data. Minor disagreements that exist are consistent with extrapolations to light nuclides of generally accepted formulations of compound-nucleus capture. We also discuss the channel-capture approximation which is, in general, a good representation of these cross sections in heavier nuclei particularly if the scattering lengths are not different from the corresponding potential radii. We also draw attention to cases where the use of this formula leads to inaccurate predictions. 9 refs., 1 fig., 2 tab

  14. Combined electron capture and infrared multiphoton dissociation for multistage MS/MS in a Fourier transform ion cyclotron resonance mass spectrometer.

    Science.gov (United States)

    Håkansson, Kristina; Chalmers, Michael J; Quinn, John P; McFarland, Melinda A; Hendrickson, Christopher L; Marshall, Alan G

    2003-07-01

    We have mounted a permanent on-axis dispenser cathode electron source inside the magnet bore of a 9.4-T Fourier transform ion cyclotron resonance mass spectrometer. This configuration allows electron capture dissociation (ECD) to be performed reliably on a millisecond time scale. We have also implemented an off-axis laser geometry that enables simultaneous access to ECD and infrared multiphoton dissociation (IRMPD). Optimum performance of both fragmentation techniques is maintained. The analytical utility of performing either ECD or IRMPD on a given precursor ion population is demonstrated by structural characterization of several posttranslationally modified peptides: IRMPD of phosphorylated peptides results in few backbone (b- and y-type) cleavages, and product ion spectra are dominated by neutral loss of H3PO4. In contrast, ECD provides significantly more backbone (c- and z*-type) cleavages without loss of H3PO4. For N-glycosylated tryptic peptides, IRMPD causes extensive cleavage of the glycosidic bonds, providing structural information about the glycans. ECD cleaves all backbone bonds (except the N-terminal side of proline) in a 3-kDa glycopeptide with no saccharide loss. However, only a charge-reduced radical species and some side chain losses are observed following ECD of a 5-kDa glycopeptide from the same protein. An MS3 experiment involving IR laser irradiation of the charge-reduced species formed by electron capture results in extensive dissociation into c- and z-type fragment ions. Mass-selective external ion accumulation is essential for the structural characterization of these low-abundance (modified) peptides. PMID:12964777

  15. Radiative capture of nucleons at astrophysical energies with single-particle states

    International Nuclear Information System (INIS)

    Radiative capture of nucleons at energies of astrophysical interest is one of the most important processes for nucleosynthesis. The nucleon capture can occur either by a compound nucleus reaction or by a direct process. The compound reaction cross sections are usually very small, especially for light nuclei. The direct capture proceeds either via the formation of a single-particle resonance or a non-resonant capture process. In this work we calculate radiative capture cross sections and astrophysical S-factors for nuclei in the mass region A<20 using single-particle states. We carefully discuss the parameter fitting procedure adopted in the simplified two-body treatment of the capture process. Then we produce a detailed list of cases for which the model works well. Useful quantities, such as spectroscopic factors and asymptotic normalization coefficients, are obtained and compared to published data.

  16. Analysis of the volatile compounds in Senecio scandens Buch-Ham by gas chromatography-tandem mass spectrometry based on diversified scan technologies.

    Science.gov (United States)

    Li, Sensen; Su, Yue; Guo, Yinlong

    2011-01-01

    Static headspace gas chromatography-tandem mass spectrometry was used to identify volatile compounds from Senecio scandens Buch-Ham. The elemental composition of compounds was confirmed by exploiting the tandem mass spectra of isotopic peaks from the precursor ion. Some isomers were well distinguished by the diversified scan technologies of tandem mass spectrometry (MS/MS). The MS/MS included a product ion scan, a precursor ion scan and a neutral loss scan. The results showed that 46 volatile compounds were completely identified, and the great of majority compounds were α-pinene (11.93%), n-caproaldehyde (9.02%) and dehydrosabinene (6.22%). This qualitative method is convenient and accurate and can be considered as a complementary identification method for the qualitative analysis of volatile compounds in complex samples. PMID:22006636

  17. Identification of microorganisms based on headspace analysis of volatile organic compounds by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Boots, A W; Smolinska, A; van Berkel, J J B N; Fijten, R R R; Stobberingh, E E; Boumans, M L L; Moonen, E J; Wouters, E F M; Dallinga, J W; Van Schooten, F J

    2014-06-01

    The identification of specific volatile organic compounds (VOCs) produced by microorganisms may assist in developing a fast and accurate methodology for the determination of pulmonary bacterial infections in exhaled air. As a first step, pulmonary bacteria were cultured and their headspace analyzed for the total amount of excreted VOCs to select those compounds which are exclusively associated with specific microorganisms. Development of a rapid, noninvasive methodology for identification of bacterial species may improve diagnostics and antibiotic therapy, ultimately leading to controlling the antibiotic resistance problem. Two hundred bacterial headspace samples from four different microorganisms (Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus and Klebsiella pneumoniae) were analyzed by gas chromatography-mass spectrometry to detect a wide array of VOCs. Statistical analysis of these volatiles enabled the characterization of specific VOC profiles indicative for each microorganism. Differences in VOC abundance between the bacterial types were determined using ANalysis of VAriance-principal component analysis (ANOVA-PCA). These differences were visualized with PCA. Cross validation was applied to validate the results. We identified a large number of different compounds in the various headspaces, thus demonstrating a highly significant difference in VOC occurrence of bacterial cultures compared to the medium and between the cultures themselves. Additionally, a separation between a methicillin-resistant and a methicillin-sensitive isolate of S. aureus could be made due to significant differences between compounds. ANOVA-PCA analysis showed that 25 VOCs were differently profiled across the various microorganisms, whereas a PCA score plot enabled the visualization of these clear differences between the bacterial types. We demonstrated that identification of the studied microorganisms, including an antibiotic susceptible and resistant S. aureus substrain

  18. Mass spectral analysis of picomolar amounts of compounds isolated from photosynthetic bacteria

    International Nuclear Information System (INIS)

    252Cf-plasma desorption mass spectrometry (PDMS) is performed with solid samples bombarded by MeV fission fragments. The emission of ions from the sample forms a mass spectrum characterized by parent and fragment ions of even thermally labile molecules. The analysis mode of 252Cf-PDMS is time-of-flight. Compared to quadrapole and sector-field instruments, time-of-flight has much higher sensitivity, an unlimited mass range, high transmission, and simultaneous detection of all ion masses. Because of the high sensitivity and other favorable characteristics of 252Cf-PDMS, nanomolar and picomolar amounts of biomolecules can be easily analyzed. In the course of studying and modelling the photosynthetic photoreaction center of green plants and bacteria, it has become apparent that the composition and identity and organization of the photoreaction center is important to understanding the photosynthetic apparatus. Moreover, for any model system to be valid it is important to know the identity and amount of components present in the model system. The possibility of more than one type of a similar component in the reaction center raises questions about the function for that component in the reaction center

  19. Gas chromatographic-mass spectrometric analysis of tar compounds formed during pyrolysis of rice husks

    NARCIS (Netherlands)

    Haanappel, V.A.C.; Stevens, T.W.; Hovestad, A.; Skolnik, V.; Visser, R.

    1991-01-01

    Pyrolysis of agricultural waste to produce fuel gas involves formation of tars as noxious by-products. In this paper the qualitative analysis of tars formed during pyrolysis of rice husks is presented, based on identification by gas chromatography—mass spectrometry and interpolation of retention tim

  20. Light-controlled mass formation of aggregates of molecules in organic compounds

    Institute of Scientific and Technical Information of China (English)

    Tariel D.Ebralidze; Nadia A.Ebralidze; Giorgi A.Mumladze; Enriko S.Kitsmarishvili

    2009-01-01

    During the mass formation of aggregates of molecules in a gelatin film dyed with the mixture of chrysophenine and acridine yellow dyes,photo-reorientation,photo-disorientation,and photo-orientation of the molecules are observed.Based on these observations,the photo-induction of granular aniso tropy may be realized.

  1. Photoionization mass spectrometric studies of selected compounds in a molecular beam

    Energy Technology Data Exchange (ETDEWEB)

    Trott, W.M.

    1979-03-01

    Photoionization efficiency curves have been measured at moderate to high resolution for several species produced in supersonic molecular beams of acetone, acetone-d/sub 6/ and CS/sub 2/. The molecular beam photoionization mass spectrometer which has been assembled for this work is described. The performance of this instrument has been characterized by a number of experiments and calculations.

  2. Search for neutrinos from annihilation of captured low-mass dark matter particles in the Sun by Super-Kamiokande

    CERN Document Server

    :,; Abe, K; Haga, Y; Hayato, Y; Iyogi, K; Kameda, J; Kishimoto, Y; Miura, M; Moriyama, S; Nakahata, M; Nakano, Y; Nakayama, S; Sekiya, H; Shiozawa, M; Suzuki, Y; Takeda, A; Tomura, T; Wendell, R A; Irvine, T; Kajita, 2 T; Kametani, I; Kaneyuki, 2 K; Lee, K P; Nishimura, Y; Okumura, 2 K; McLachlan, T; Labarga, 2 L; Kearns, E; Raaf, J L; Stone, 4 J L; Sulak, L R; Berkman, 4 S; Tanaka, 5 H A; Tobayama, 5 S; Goldhaber, M; Carminati, G; Kropp, W R; Mine, S; Renshaw, A; Smy, M B; Sobel, H W; Ganezer, K S; Hill, J; Hong, N; Kim, J Y; Lim, I T; Akiri, T; Himmel, A; Scholberg, K; Walter, C W; Wongjirad, T; Ishizuka, T; Tasaka, S; Jang, J S; Learned, J G; Matsuno, S; Smith, S N; Hasegawa, T; Ishida, T; Ishii, T; Kobayashi, T; Nakadaira, T; Nakamura, K; Oyama, Y; Sakashita, K; Sekiguchi, T; Tsukamoto, T; Suzuki, A T; Takeuchi, Y; Bronner, C; Hirota, S; Huang, K; Ieki, K; Ikeda, M; Kikawa, T; Minamino, A; Nakaya, T; Suzuki, K; Takahashi, S; Fukuda, Y; Itow, Y; Mitsuka, G; Mijakowski, P; Hignight, J; Imber, J; Jung, C K; Yanagisawa, C; Ishino, H; Kibayashi, A; Koshio, Y; Mori, T; Sakuda, M; Yano, T; Kuno, Y; Tacik, R; Kim, S B; Okazawa, H; Choi, Y; Nishijima, K; Koshiba, M; Totsuka, Y; Yokoyama, M; Martin, J F; de Perio, P; Konaka, A; Wilking, M J; Chen, S; Zhang, Y; Wilkes, R J

    2015-01-01

    Super-Kamiokande (SK) can search for weakly interacting massive particles (WIMPs) by detecting neutrinos produced from WIMP annihilations occurring inside the Sun. In this analysis, we include neutrino events with interaction vertices in the detector in addition to upward-going muons produced in the surrounding rock. Compared to the previous result, which used the upward-going muons only, the signal acceptances for light (few-GeV/$c^2$ $\\sim$ 200-GeV/$c^2$) WIMPs are significantly increased. We fit 3903 days of SK data to search for the contribution of neutrinos from WIMP annihilation in the Sun. We found no significant excess over expected atmospheric-neutrino background and the result is interpreted in terms of upper limits on WIMP-nucleon elastic scattering cross sections under different assumptions about the annihilation channel. We set the current best limits on the spin-dependent (SD) WIMP-proton cross section for WIMP masses below 200 GeV/$c^2$ (at 10 GeV/$c^2$, 1.49$\\times 10^{-39}$ cm$^2$ for $\\chi\\c...

  3. Combined infrared multiphoton dissociation and electron capture dissociation with a hollow electron beam in Fourier transform ion cyclotron resonance mass spectrometry.

    Science.gov (United States)

    Tsybin, Youri O; Witt, Matthias; Baykut, Gökhan; Kjeldsen, Frank; Håkansson, Per

    2003-01-01

    An electron injection system based on an indirectly heated ring-shaped dispenser cathode has been developed and installed in a 7 Tesla Fourier transform ion cyclotron resonance (FTICR) mass spectrometer. This new hardware design allows high-rate electron capture dissociation (ECD) to be carried out by a hollow electron beam coaxial with the ion cyclotron resonance (ICR) trap. Infrared multiphoton dissociation (IRMPD) can also be performed with an on-axis IR-laser beam passing through a hole at the centre of the dispenser cathode. Electron and photon irradiation times of the order of 100 ms are required for efficient ECD and IRMPD, respectively. As ECD and IRMPD generate fragments of different types (mostly c, z and b, y, respectively), complementary structural information that improves the characterization of peptides and proteins by FTICR mass spectrometry can be obtained. The developed technique enables the consecutive or simultaneous use of the ECD and IRMPD methods within a single FTICR experimental sequence and on the same ensemble of trapped ions in multistage tandem (MS/MS/MS or MS(n)) mass spectrometry. Flexible changing between ECD and IRMPD should present advantages for the analysis of protein digests separated by liquid chromatography prior to FTICRMS. Furthermore, ion activation by either electron or laser irradiation prior to, as well as after, dissociation by IRMPD or ECD increases the efficiency of ion fragmentation, including the w-type fragment ion formation, and improves sequencing of peptides with multiple disulfide bridges. The developed instrumental configuration is essential for combined ECD and IRMPD on FTICR mass spectrometers with limited access into the ICR trap. PMID:12872281

  4. Tandem Extraction/Liquid Chromatography-Mass Spectrometry Protocol for the Analysis of Acrylamide and Surfactant-related Compounds in Complex Aqueous Environmental Samples

    Science.gov (United States)

    The development of a liquid chromatography‐mass spectrometry (LC‐MS)‐based strategy for the detection and quantitation of acrylamide and surfactant‐related compounds in aqueous complex environmental samples.

  5. Selective capture and rapid identification of Panax notoginseng metabolites in rat faeces by the integration of magnetic molecularly imprinted polymers and high-performance liquid chromatography coupled with orbitrap mass spectrometry.

    Science.gov (United States)

    Cai, Qizhi; Yang, Zaiyue; Chen, Ning; Zhou, Xuemin; Hong, Junli

    2016-07-15

    In the present work, an advanced pretreatment method magnetic molecular imprinted polymers-dispersive solid phase extraction (MMIPs-DSPE) combined with the high sensitivity LTQ-Orbitrap mass spectrometry was applied to the complicated metabolites analysis of Traditional Chinese Medicines (TCMs) in complex matrices. The ginsenoside Rb1 magnetic molecular imprinted polymers (Rb1-MMIPs) were successfully synthesized for specific recognition and selective enrichment of Panax notoginseng saponin metabolites in rat faeces. The polymers were prepared by using Fe3O4@SiO2 as the supporting material, APTES as the functional monomer and TEOS as the cross-linker. The Rb1-MMIPs showed quick separation (10.8 emu/g), large adsorption capacity (636μmol/g), high selectivity and fast binding kinetics (25min). Dispersion solid-phase extraction using Rb1-MMIPs (Rb1-MMIPs-DSPE) integrated with LTQ-Orbitrap MS was applied to fish out and identify saponin metabolites from rat faeces, and totally 58 related compounds were detected within 20min, including 26 PPD-group and 32 PPT-group notoginsenoside metabolites. Parallel tests showed that Rb1-MMIPs-DSPE obtained the lowest matrix effects of 0.98-14.84% and captured the largest number of structural analogues compared with traditional pretreatment methods organic solvent extraction (OSE) and solid phase extraction (SPE). PMID:27295967

  6. Isolation and identification of Phenolic compounds by HPLC and Electrospray Ionization Mass Spectrometry of Svensonia Hyderobadensis ? A Rare Medicinal Plant Taxon

    OpenAIRE

    Linga Rao M; Savithramma N

    2014-01-01

    The impetus for developing analytical methods for phenolic compounds in natural products has proved to be multifaceted. Hence the present study intended to isolate phenolic compounds from leaves of Svensonia hyderobadensis by using 70% acetone and poly vinyl poly pyrrolidone (PVPP); and characterized by U.V. Visible spectrometry, High performance liquid chromatography/ electrospray ionization mass spectrometry. Total 82 phenolic compounds were obtained at both positive and negative ion modes ...

  7. Nontargeted Identification of the Phenolic and Other Compounds of Saraca asoca by High Performance Liquid Chromatography-Positive Electrospray Ionization and Quadrupole Time-of-Flight Mass Spectrometry

    OpenAIRE

    Ashwani Mittal; Preeti Kadyan; Anjum Gahlaut; Rajesh Dabur

    2013-01-01

    High performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometer was used for separation and identification of phenolic and other compounds in the water extracts of Saraca asoca (Roxb.), De. Wilde. The aim of the study was to identify and evaluate the distribution of phenolic compounds in the different parts of the plant. The identity of compounds was established through the comparison with standards and characteristic base peaks as well as other daughter ions. ...

  8. Extraction and Characterization of Phenolic Compounds from Rose Hip (Rosa canina L.) Using Liquid Chromatography Coupled with Electrospray Ionization - Mass Spectrometry

    OpenAIRE

    Stănilă, Andreea; Diaconeasa, Zoriţa; Roman, Ioana; Nicușor SIMA; Dănuț MĂNIUȚIU; Alin ROMAN; Rodica SIMA

    2015-01-01

    Wild berry are a rich of natural compounds which provide them high antioxidant potential. The compounds which provide them these proprieties are known to be vitamins, flavonoids, anthocyanins and phenolic acids. The aim of this study was to extract and characterize bioactive compounds from rose hip (Rosa canina L.) currently found in Romania. A qualitative high-performance liquid chromatography coupled with electrospray ionization mass spectrometric (ESI-MS) detection in positive ion mode has...

  9. Gas chromatographic-mass spectrometric analysis of tar compounds formed during pyrolysis of rice husks

    OpenAIRE

    Haanappel, V.A.C.; Stevens, T.W.; Hovestad, A.; Skolnik, V.; Visser, R.

    1991-01-01

    Pyrolysis of agricultural waste to produce fuel gas involves formation of tars as noxious by-products. In this paper the qualitative analysis of tars formed during pyrolysis of rice husks is presented, based on identification by gas chromatography—mass spectrometry and interpolation of retention times on a polyaromatic hydrocarbon index scale. The influence of some reaction parameters on product formation is briefly discussed.

  10. Reduced matrix effects for anionic compounds with paired ion electrospray ionization mass spectrometry.

    Science.gov (United States)

    Guo, Hongyue; Breitbach, Zachary S; Armstrong, Daniel W

    2016-03-17

    It is well-known that matrix effects in high performance liquid chromatography coupled to electrospray ionization mass spectrometry (HPLC-ESI-MS) can seriously compromise quantitative analysis and affect method reproducibility. Paired ion electrospray ionization (PIESI) mass spectrometry is an approach for analyzing ultra-low levels of anions in the positive ion mode. This approach uses a structurally optimized ion pairing reagent to post-column associate with the anionic analyte, subsequently forming positively charged complexes. These newly formed complex ions are often more surface-active as compared to either the native anion or the ion pairing reagent. No studies have examined whether or not the PIESI approach mitigates matrix effects. Consequently, a controlled study was done using five analytes in highly controlled and reproducible synthetic groundwater and urine matrices. In addition, two different mass spectrometers (linear ion trap and triple quadrupole) were used. Compared to the negative ion mode, the PIESI-MS approach was less susceptible to matrix effects when performed on two different MS platforms. Using PIESI-MS, less dilution of the sample is needed to eliminate ionization suppression which, in turn, permits lower limits of detection and quantitation. PMID:26920775

  11. Chiral Signatures of Anthropogenic Semi-Volatile Organic Compounds in Asian, trans- Pacific, and Pacific Northwestern Air Masses

    Science.gov (United States)

    Genualdi, S.; Primbs, T.; Bidleman, T.; Jantunen, L.; Simonich, S.

    2006-12-01

    The goal of this research is to use the chiral signatures of Semi-Volatile Organic Compounds (SOCs) to distinguish between new and old sources in Asian, trans-Pacific, and regional air masses. During 2004, a six week air sampling campaign was conducted at a remote site in Okinawa, Japan to determine the chemical composition of Eurasian air masses. During 2003 and 2004, high volume air samples were collected at three different locations in the Pacific Northwest of the United States. These sampling locations were; Mary's Peak Observatory (MPO) located at 1250m in the Oregon Coast Range, Mt. Bachelor located at 2800m in Oregon's Cascade Range, and Cheeka Peak Observatory (CPO) located at 500m in the state of Washington. The air samples consisted of both polyurethane foam and XAD-2 resin to collect the gas phase SOCs, and glass fiber filters to collect the particulate phase SOCs. The samples were extracted using accelerated solvent extraction and enantiomer fractions were determined using GCMS-ECNI with the use of a BGB Analytik chiral column. The chiral SOCs, á-Hexachlorocyclohexane, cis and trans chlordane, heptachlor epoxide, and o'p' DDT, were measured, the enantiomer ratios were determined, and potential new and historical sources of these compounds were identified.

  12. Conversion of 3-nitrotyrosine to 3-aminotyrosine residues facilitates mapping of tyrosine nitration in proteins by electrospray ionization-tandem mass spectrometry using electron capture dissociation.

    Science.gov (United States)

    Guo, Jia; Prokai, Laszlo

    2012-12-01

    Protein tyrosine nitration is associated with oxidative stress and various human diseases. Tandem mass spectrometry has been the method of choice for the identification and localization of this posttranslational modification to understand the underlying mechanisms and functional consequences. Due to the electron predator effect of the nitro group limiting fragmentation of the peptide backbone, electron-based dissociation has not been applicable, however, to nitrotyrosine-containing peptides. A straightforward conversion of the nitrotyrosine to the aminotyrosine residues is introduced to address this limitation. When tested with nitrated ubiquitin and human serum albumin as model proteins in top-down and bottom-up approaches, respectively, this chemical derivatization enhanced backbone fragmentation of the corresponding nitroproteins and nitropeptides by electron capture dissociation (ECD). Increased sequence coverage has been obtained by combining in the bottom-up strategy the conversion of nitrotyrosine to aminotyrosine and introducing, in addition to trypsin, a further digesting enzyme of complementary specificity, when protein nitration was mapped by liquid chromatography-electrospray ionization tandem mass spectrometry using both collision-induced dissociation (CID) and ECD. PMID:23280749

  13. Occurrence of pharmaceutical compounds in urban wastewater: Removal, mass load and environmental risk after a secondary treatment-A review

    Energy Technology Data Exchange (ETDEWEB)

    Verlicchi, P., E-mail: paola.verlicchi@unife.it [Dept. of Engineering, University of Ferrara, Via Saragat 1, I-44122 Ferrara (Italy); Terra and AcquaTech Technopoles, Via Borsari 46, I-44121 Ferrara (Italy); Al Aukidy, M., E-mail: mustafakether.alaukidi@unife.it [Dept. of Engineering, University of Ferrara, Via Saragat 1, I-44122 Ferrara (Italy); Zambello, E., E-mail: elena.zambello@unife.it [Dept. of Engineering, University of Ferrara, Via Saragat 1, I-44122 Ferrara (Italy); Terra and AcquaTech Technopoles, Via Borsari 46, I-44121 Ferrara (Italy)

    2012-07-01

    This review focuses on 118 pharmaceuticals, belonging to seventeen different therapeutic classes, detected in raw urban wastewater and effluent from an activated sludge system, a usual treatment adopted for urban wastewaters worldwide prior to final discharge into surface water bodies. Data pertaining to 244 conventional activated sludge systems and 20 membrane biological reactors are analysed and the observed ranges of variability of each selected compound in their influent and effluent reported, with particular reference to the substances detected most frequently and in higher concentrations. A snapshot of the ability of these systems to remove such compounds is provided by comparing their global removal efficiencies for each substance. Where possible, the study then evaluates the average daily mass load of the majority of detected pharmaceuticals exiting the secondary treatment step. The final part of the review provides an assessment of the environmental risk posed by their presence in the secondary effluent by means of the risk quotient that is the ratio between the average pharmaceutical concentration measured in the secondary effluent and the predicted no-effect concentration. Finally, mass load rankings of the compounds under review are compared with those based on their risk level. This analysis shows that the highest amounts discharged through secondary effluent pertain to one antihypertensive, and several beta-blockers and analgesics/anti-inflammatories, while the highest risk is posed by antibiotics and several psychiatric drugs and analgesics/anti-inflammatories. These results are reported with a view to aiding scientists and administrators in planning measures aiming to reduce the impact of treated urban wastewater discharge into surface water bodies. - Highlights: Black-Right-Pointing-Pointer The review refers to 118 pharmaceuticals occurring in raw and treated wastewaters. Black-Right-Pointing-Pointer Data from 264 municipal WWTPs with a CAS or an

  14. Determination of Volatile Compounds in Four Commercial Samples of Japanese Green Algae Using Solid Phase Microextraction Gas Chromatography Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Masayoshi Yamamoto

    2014-01-01

    Full Text Available Green algae are of great economic importance. Seaweed is consumed fresh or as seasoning in Japan. The commercial value is determined by quality, color, and flavor and is also strongly influenced by the production area. Our research, based on solid phase microextraction gas chromatography mass spectrometry (SPME-GC-MS, has revealed that volatile compounds differ intensely in the four varieties of commercial green algae. Accordingly, 41 major volatile compounds were identified. Heptadecene was the most abundant compound from Okayama (Ulva prolifera, Tokushima (Ulva prolifera, and Ehime prefecture (Ulva linza. Apocarotenoids, such as ionones, and their derivatives were prominent volatiles in algae from Okayama (Ulva prolifera and Tokushima prefecture (Ulva prolifera. Volatile, short chained apocarotenoids are among the most potent flavor components and contribute to the flavor of fresh, processed algae, and algae-based products. Benzaldehyde was predominant in seaweed from Shizuoka prefecture (Monostroma nitidum. Multivariant statistical analysis (PCA enabled simple discrimination of the samples based on their volatile profiles. This work shows the potential of SPME-GC-MS coupled with multivariant analysis to discriminate between samples of different geographical and botanical origins and form the basis for development of authentication methods of green algae products, including seasonings.

  15. RESEARCH OF SOPHORA JAPONICA L. FLOWER BUDS VOLATILE COMPOUNDS WITH GAS-CHROMATOGRAPHY/MASS- SPECTROMETRY METHOD

    Directory of Open Access Journals (Sweden)

    Cholak I.S.

    2013-10-01

    Full Text Available This work represents the results of the research ofessential oil contained in Sophora japonica L. flowerbuds volatile compounds collected during the nextstages of their development: green flower buds, formedflower buds and the beginning of flower buds opening.Essential oil assay content in Sophora japonica L.flower buds was determined with hydrodistillationmethod. Content of essential oil in the raw material isless than 0,1%. Qualitative composition and assaycontent of Sophora japonica L. flower buds essential oilconstituents were determined with chromato-massspectrometry method. In consequence of the research 80constituents were identified in Sophora japonica L.flower buds out of which 61 substances are during thegreen flower buds and beginning of flower budsopening stages, 66 substances are during formed flowerbuds stage. Substances are represented by aliphatic andcyclic terpenoids, their alcohols and ketones. Mostvolatile substances were extracted on the stage offormed buds.

  16. Report on three aliphatic dimethylarsinoyl compounds as common minor constituents in marine samples. An investigation using high-performance liquid chromatography inductively coupled plasma mass spectrometry and electrospray ionisation tandem mass spectrometry

    DEFF Research Database (Denmark)

    Sloth, Jens Jørgen; Larsen, Erik Huusfeldt; Julshamn, K.

    2005-01-01

    chromatography/inductively coupled plasma mass spectrometry (HPLC/ICPMS). Eluate fractions from the HPLC/ICPMS analyses containing the compounds in question were collected and subjected to analysis by electrospray ionisation tandem mass spectrometry (ESI-MS/MS), which provided supportive evidence for the...... DMAA and DMAE supports a proposed biosynthesis of arsenobetaine (AB) from dimethylarsinoylribosides. Alternative proposals, which explain the presence of the compounds in marine samples, are addressed briefly in the paper....

  17. Measurement of light charged particles in the decay channels of medium-mass excited compound nuclei

    Directory of Open Access Journals (Sweden)

    Valdré S.

    2014-03-01

    Indeed, in this mass region (A ~ 100 models predict that shape transitions can occur at high spin values and relatively scarce data exist in the literature about coincidence measurements between evaporation residues and light charged particles. Signals of shape transitions can be found in the variations of the lineshape of high energy gamma rays emitted from the de-excitation of GDR states gated on different region of angular momenta. For this purpose it is important to keep under control the FE and FF processes, to regulate the statistical model parameters and to control the onset of possible pre-equilibrium emissions from 300 to 600 MeV bombarding energy.

  18. Analysis of odour compounds from scented consumer products using gas chromatography-mass spectrometry and gas chromatography-olfactometry.

    Science.gov (United States)

    Bartsch, Jennifer; Uhde, Erik; Salthammer, Tunga

    2016-01-21

    Scented consumer products are being bought in increasing amounts and gaining more popularity. There is, however, relatively little information available about their ingredients, emissions and allergenic potential. Frequently, a mixture of different fragrance substances and not solely an individual substance contributes to the overall desired smell. The aim of this study was to investigate the odorous volatile organic compounds (OVOCs) in consumer products containing fragrances. Over 44 products were selected: various scented candles, printing products with different scent types and other products types particularly meant to be used indoors. Measurements were carried out in a desiccator. Air samples were collected on thermal desorption tubes to determine the released fragrance substances by means of gas chromatography-mass spectrometry (GC-MS). Moreover, gas chromatography-olfactometry (GC-O) was used to obtain sensory data and to ensure no important odorant was overlooked. Using both methods it was possible to distinguish between odour active and inactive compounds and subsequently to identify almost 300 different odorants across all scented products. Besides the advantage of differentiation, as the human nose is a very sensitive detector, GC-O was found to be a useful tool for detecting traces and chosen target compounds. One focus in this study lay on the 26 EU-regulated fragrance allergens to prove their relevance in scented consumer goods. In total, 18 of them were identified, with at least one substance being present in almost every product. Benzyl alcohol, cinnamaldehyde, citronellol, eugenol, linalool and limonene were the prevalently detected allergens. Particularly linalool and limonene were observed in over 50% of the products. In addition, eugenol appeared to be one of the most frequently detected compounds in trace-level concentrations in the candle emissions. PMID:26724768

  19. Vapour pressures of selected organic compounds down to 1 mPa, using mass-loss Knudsen effusion method

    International Nuclear Information System (INIS)

    Graphical abstract: - Highlights: • A recently described mass-loss Knudsen apparatus was used for measurements of vapour pressures down to around 1 mPa. • Complementary calorimetric studies were performed in a Calvet-type calorimeter. • New vapour pressures are given for benzoic acid and benzanthrone, in ranges in which no consistent data existed. • Vapour pressures for solid n-octadecane are presented, correcting existing values from literature. - Abstract: A recently developed Knudsen effusion apparatus was improved and used for measurements of vapour pressures of selected organic compounds. Calorimetric studies were conducted using a Calvet-type calorimeter, complementing the information obtained for the vapour pressures and facilitating the modelling and analysis of the data. Vapour pressures of benzoic acid, a reference substance, were determined at temperatures between 269 K and 317 K, corresponding to a pressure range from 2 mPa to 1 Pa, extending the range of results available in the literature to lower pressures. Benzanthrone was studied between temperatures 360 K and 410 K (5 mPa–1 Pa) in order to test the apparatus at higher temperatures. Values presented in the literature for the vapour pressure of solid n-octadecane, one of the most promising compounds to be used as “phase change material” for textile applications, were found inconsistent with the triple point of the substance. Sublimation pressures were measured for this compound between T = 286 K and 298 K (2–20 mPa) allowing the correction of the existing values. Finally, vapour pressures of diphenyl carbonate, a compound of high industrial relevance for its use in the production of polycarbonates, were determined from T = 302 K to 332 K (0.02–1 Pa)

  20. Proteomic analysis of prolactinoma cells by immuno-laser capture microdissection combined with online two-dimensional nano-scale liquid chromatography/mass spectrometry

    Directory of Open Access Journals (Sweden)

    Chen Luping

    2010-01-01

    Full Text Available Abstract Background Pituitary adenomas, the third most common intracranial tumor, comprise nearly 16.7% of intracranial neoplasm and 25%-44% of pituitary adenomas are prolactinomas. Prolactinoma represents a complex heterogeneous mixture of cells including prolactin (PRL, endothelial cells, fibroblasts, and other stromal cells, making it difficult to dissect the molecular and cellular mechanisms of prolactin cells in pituitary tumorigenesis through high-throughout-omics analysis. Our newly developed immuno-laser capture microdissection (LCM method would permit rapid and reliable procurement of prolactin cells from this heterogeneous tissue. Thus, prolactin cell specific molecular events involved in pituitary tumorigenesis and cell signaling can be approached by proteomic analysis. Results Proteins from immuno-LCM captured prolactin cells were digested; resulting peptides were separated by two dimensional-nanoscale liquid chromatography (2D-nanoLC/MS and characterized by tandem mass spectrometry. All MS/MS spectrums were analyzed by SEQUEST against the human International Protein Index database and a specific prolactinoma proteome consisting of 2243 proteins was identified. This collection of identified proteins by far represents the largest and the most comprehensive database of proteome for prolactinoma. Category analysis of the proteome revealed a widely unbiased access to various proteins with diverse functional characteristics. Conclusions This manuscript described a more comprehensive proteomic profile of prolactinomas compared to other previous published reports. Thanks to the application of immuno-LCM combined with online two-dimensional nano-scale liquid chromatography here permitted identification of more proteins and, to our best knowledge, generated the largest prolactinoma proteome. This enlarged proteome would contribute significantly to further understanding of prolactinoma tumorigenesis which is crucial to the management of

  1. Control of radioactive wastes and coupling of neutron/gamma measurements: use of radiative capture for the correction of matrix effects that penalize the fissile mass measurement by active neutron interrogation; Controle des dechets radioactifs et couplage de mesures neutron/gamma: exploitation de la capture radiative pour corriger les effets de matrice penalisant la mesure de la masse fissile par interrogation neutronique active

    Energy Technology Data Exchange (ETDEWEB)

    Loche, F

    2006-10-15

    In the framework of radioactive waste drums control, difficulties arise in the nondestructive measurement of fissile mass ({sup 235}U, {sup 239}Pu..) by Active Neutron Interrogation (ANI), when dealing with matrices containing materials (Cl, H...) influencing the neutron flux. The idea is to use the neutron capture reaction (n,{gamma}) to determine the matrix composition to adjust the ANI calibration coefficient value. This study, dealing with 118 litres, homogeneous drums of density less than 0,4 and composed of chlorinated and/or hydrogenated materials, leads to build abacus linking the {gamma} ray peak areas to the ANI calibration coefficient. Validation assays of these abacus show a very good agreement between the corrected and true fissile masses for hydrogenated matrices (max. relative standard deviation: 23 %) and quite good for chlorinated and hydrogenated matrices (58 %). The developed correction method improves the measured values. It may be extended to 0,45 density, heterogeneous drums. (author)

  2. From storage ion trap of an 'in-flight capture' type for precise mass measurement of radioactive nuclei to mass selector of weight amounts of stable isotopes and to effective accumulator-collider of accelerated fusion hydrogen nuclei

    International Nuclear Information System (INIS)

    Full text: Data on nuclear masses provide a basis for creating and testing various nuclear models. A tandem system comprised of the U-400M cyclotron, the COMBAS magnetic separator and the mass spectrometric ion trap of a 'in-flight capture' type is considered as a complex for producing of the short -lived nuclei by heavy ions in fragmentation reactions and for precise mass measurement of this nuclei. In-flight transportation of the recoiled nuclei to the magnetic solenoid of the ionic trap and transformation their longitudinal kinetic energy into an azimuth rotation arc produced by the fringing magnetic field according to Bush's theorem at the off axial input. Confinement and accumulation of the rotating ions in the trap are produced by using their reflecting by the electrostatic field of the final end cap electrode of the volume quadrupole and their repelling by a magnetic valve located at the entrance. The development of mass spectroscopic ion traps of a new tape resulted in a efficient method for selecting stable isotopes of non volatile chemical elements in the weight amounts analogously needed for physical and technical aims. The system uses ionic-cyclotron resonance in homogenous magnetic and volume quadrupole electric fields. In our case there are used general rotating excitation of the accelerated ions by the off axial input in the solenoid and their high frequency electric resonance cooling. There are axial transparency volume electric quadrupole with axial GZR >0 gradients (in the Penning trap GZ>0 and GR2 H+3H=4He+n having a very large resonance cross section at very low energy (63.0 keV in the centre-of-mass frame) in the merging collisions

  3. APPLICABILITY OF THE MASS ACTION LAW IN COMBINATION WITH THE COEXISTENCE THEORY OF METALLIC MELTS INVOLVING COMPOUND TO BINARY METALLIC MELTS

    Institute of Scientific and Technical Information of China (English)

    J. Zhang

    2002-01-01

    Based on the atomicity and molecularity as well as the consistency of thermodynamicproperties and activities of metallic melts with their structures, the coexistence the-ory of metallic melts structure involving compound has been suggested. According tothis theory, the calculating models of mass action concentrations for different binarymetallic melts have been formulated. The calculated mass action concentrations agreewell with corresponding measured activities, which confirms that the suggested theorycan reflect the structural characteristics of metallic melts involving compound and thatthe mass action law is widely applicable to this kind of metallic melts.

  4. Detection of Volatile Aroma Compounds of Morchella by Headspace Gas Chromatography Mass Spectrometry (HS-GC/MS

    Directory of Open Access Journals (Sweden)

    Hatira TAŞKIN

    2013-05-01

    Full Text Available   This study was conducted at the Horticulture Department of Çukurova University, Adana, Turkey, in 2010 to determine the volatile aroma compounds of Morchella mushroom. Fresh samples of Morchella esculenta (Sample 1 and Morchella elata (Sample 2 were collected from Çanakkale (Sample 1 and Mersin (Sample 2 provinces in Turkey in the spring of 2010. Volatile aroma compounds were analyzed by headspace gas chromatography mass spectrometry (HS-GC/MS. A total of 31 aroma compounds were identified in the 2 analyzed samples: 7 alcohols, 7 esters, 7 ketones, 3 acids, 2 aldehydes, 1 terpene, phenol, 1-propanamine, geranyl linalool, and quinoline. Seventeen aroma components were identified in Sample 1, and 18 compounds were found in Sample 2. Phenol was determined as the major aroma compound in both Sample 1 and Sample 2, at 50.888% and 58.293% content, respectively. Alcohols, especially 1-octen-3-ol, were detected as the second major aroma components in Sample 1 and Sample 2, at 15.500% and 5.660% content, respectively. Carbamic acid, methyl ester was found only in Sample 1, at 11.379% content. The aroma components detected in the two samples differed. 1-Octadecanol; cyclooctylalcohol; trans-2-undecen-1-ol; butanoic acid, butyl ester (CAS; carbamic acid, methyl ester; 2-ethylhexyl-2-ethylhexanoate; phthalic acid, decyl isobutyl ester; 2,2,4-trimethyl-1,3-pentanediol diisobutyrate; decanal; nonanal; 7,9-di-tert-butyl-1-oxaspiro(4.5deca-6,9-diene-2,8-dione; 2,5-cyclohexadiene-1,4-dione; 2,6-bis(1,1-dimethylethyl; and trans-alpha-bisabolene were detected only in Sample 1. Ethanol; silanediol, 2-methylaminoethanol; L-alanine, ethyl ester; carbonic acid, dodecyl isobutyl ester; acetic acid; butanoic acid; 2,3,4H-pyran-4-one; 5,9-undecadien-2-one; cyclooctene; 2-cyclopenten-1-one; 1-propanamine; geranyl linalool; and quinoline were determined only in Sample 2.

  5. COMPOUND TWIN CORONAL MASS EJECTIONS IN THE 2012 MAY 17 GLE EVENT

    Energy Technology Data Exchange (ETDEWEB)

    Shen, C.; Wang, Yuming [CAS Key Laboratory of Geospace Environment, Department of Geophysics and Planetary Sciences, University of Science and Technology of China, Hefei, Anhui 230026 (China); Li, G.; Kong, X.; Hu, J. [Department of Physics and CSPAR, University of Alabama in Huntsville, Huntsville, AL 35899 (United States); Sun, X. D. [W. W. Hansen Experimental Physics Laboratory, Stanford University, Stanford, CA 94305 (United States); Ding, L. [School of Physics and Optoelectronic Engineering, Nanjing University of Information Science and Technology, Nanjing 210044 (China); Chen, Y.; Xia, L., E-mail: gang.li@uah.edu [Shandong Provincial Key Laboratory of Optical Astronomy and Solar-Terrestrial Environment, School of Space Science and Physics, Shandong University at Weihai, Weihai 264209 (China)

    2013-02-15

    We report a multiple spacecraft observation of the 2012 May 17 GLE event. Using the coronagraph observations by SOHO/LASCO, STEREO-A/COR1, and STEREO-B/COR1, we identify two eruptions resulting in two coronal mass ejections (CMEs) that occurred in the same active region and close in time ({approx}2 minutes) in the 2012 May 17 GLE event. Both CMEs were fast. Complicated radio emissions, with multiple type II episodes, were observed from ground-based stations: Learmonth and BIRS, as well as the WAVES instrument on board the Wind spacecraft. High time-resolution SDO/AIA imaging data and SDO/HMI vector magnetic field data were also examined. A complicated pre-eruption magnetic field configuration, consisting of twisted flux-tube structure, is reconstructed. Solar energetic particles (SEPs) up to several hundred MeV nucleon{sup -1} were detected in this event. Although the eruption source region was near the west limb, the event led to ground-level enhancement. The existence of two fast CMEs and the observation of high-energy particles with ground-level enhancement agrees well with a recently proposed 'twin CME' scenario.

  6. Characterisation of honeys according to their content of phenolic compounds using high performance liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Sergiel, Iwona; Pohl, Pawel; Biesaga, Magdalena

    2014-02-15

    A simple, fast and specific high performance liquid chromatography separation with an electro-spray ionisation tandem mass spectrometry detection in a negative single reaction ion monitoring scan mode was developed and used for the characterization of Polish honeys according to the content of phenolic acids, including caffeic, chlorogenic, p-coumaric, ferulic, homogentisic, p-hydroxybenzoic and vanillic acids, and flavonoids, i.e., apigenin, genistein, hesperetin, kaempferol, luteolin, rhamnetin, rutin, tricetin and quercetin. Target compounds were isolated and pre-concentrated from the honey matrix by means of the solid phase extraction using Strata X (500mg) cartridges. Analysed honeys did not contain tricetin and genistein. Hesperetin was determined for the first time in heather and linden honeys while rutin in rape honey. PMID:24128495

  7. Identification and quantitation of glycosidically bound aroma compounds in three tobacco types by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cai, Kai; Xiang, Zhangmin; Pan, Wenjie; Zhao, Huina; Ren, Zhu; Lei, Bo; Geng, Zhaoliang

    2013-10-11

    Glycosidically bound aroma compounds in three different types of tobacco were investigated. After isolation of extracts obtained by Amberlite XAD-2 adsorption and ethyl acetate elution, glycosides were analyzed after enzymatic hydrolysis by gas chromatography-mass spectrometry (GC-MS) or directly after trifluoroacetylated (TFA) derivatization by GC-MS in electron ionization (EI) and negative chemical ionization (NCI) mode. In total 21 bound aglycones were identified by β-glucosidase hydrolysis. These aglycones mainly consisted of C13-norisoprenoids, aromatic components and sesquiterpenoids. Additionally, with the aid of enzymatic hydrolysis, 15 β-d-glucopyranosides and 1 β-d-rutinoside were tentatively identified by TFA derivatization. TFA method was validated by repeatability and successfully employed to analyze different types of tobacco. Principal component analysis (PCA) was carried out on identified glycoside variables to visualize the difference between the tobacco types and the relationship between the glycoside variables and the tobacco types was established. PMID:24011421

  8. Modeling the heat and mass transfers in temperature-swing adsorption of volatile organic compounds onto activated carbons

    Energy Technology Data Exchange (ETDEWEB)

    Sylvain Giraudet; Pascaline Pre; Pierre Le Cloirec [Ecole des Mines de Nantes, Nantes (France)

    2009-02-15

    A theoretical model was built to simulate the adsorption of volatile organic compounds (VOCs) onto activated carbons in a fixed bed. This model was validated on a set of experimental data obtained for the adsorption of acetone, ethyl formate, and dichloromethane onto five commercial activated carbons. The influence of operating conditions was modeled with various VOC contents at the inlet of the adsorber and superficial velocities of the gas-phase from 0.14 to 0.28 m.s{sup -1}. Breakthrough times and maximum temperature rises were computed with a coefficient of determination of 0.988 and 0.901, respectively. The simulation was then extended to the adsorption of mixtures of VOCs. From the comparison of simulation and experimental results, the advantage of accounting for dispersions of heat and mass is shown and the importance in taking into account the temperature effect on the equilibrium data is demonstrated. 29 refs., 6 figs., 1 tab.

  9. Lunar Sulfur Capture System Project

    Data.gov (United States)

    National Aeronautics and Space Administration — The Lunar Sulfur Capture System (LSCS) is an innovative method to recover sulfur compounds from lunar soil using sorbents derived primarily from in-situ resources....

  10. Measurements of Volatile Organic Compounds Using Proton Transfer Reaction – Mass Spectrometry during the MILAGRO 2006 Campaign

    Directory of Open Access Journals (Sweden)

    E. C. Fortner

    2009-01-01

    Full Text Available Volatile organic compounds (VOCs were measured by proton transfer reaction – mass spectrometry (PTR-MS on a rooftop in the urban mixed residential and industrial area North Northeast of downtown Mexico City as part of the Megacity Initiative – Local and Global Research Observations (MILAGRO 2006 field campaign. Thirty eight individual masses were monitored during the campaign and many species were quantified including methanol, acetaldehyde, toluene, the sum of C2 benzenes, the sum of C3 benzenes, acetone, isoprene, benzene, and ethyl acetate. The VOC measurements were analyzed to gain a better understanding of the type of VOCs present in the MCMA, their diurnal patterns, and their origins. Diurnal profiles of weekday and weekend/holiday aromatic VOC concentrations showed the influence of vehicular traffic during the morning rush hours and during the afternoon hours. Plumes including elevated toluene as high as 216 parts per billion (ppb and ethyl acetate as high as 183 ppb were frequently observed during the late night and early morning hours, indicating the possibility of significant industrial sources of the two compounds in the region. Wind fields during those peak episodes revealed no specific direction for the majority of the toluene plumes but the ethyl acetate plumes arrived at the site when winds were from the Southwest or West. The PTR-MS measurements combined with other VOC measuring techniques at the field site as well as VOC measurements conducted in other areas of the Mexico City Metropolitan Area (MCMA will help to develop a better understanding of the spatial pattern of VOCs and its variability in the MCMA.

  11. Development of a matrix-assisted laser desorption ionization mass spectrometric method for rapid process-monitoring of phthalocyanine compounds

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Yi-Ting, E-mail: ytchen@mail.cgu.edu.tw [Department of Chemistry, National Tsing Hua University, Hsinchu 30013, Taiwan (China); Molecular Medicine Research Center, College of Medicine, Chang Gung University, Taoyuan 33302, Taiwan (China); Wang, Fu-Shing [Department of Chemistry, National Tsing Hua University, Hsinchu 30013, Taiwan (China); Li, Zhendong [Department of Chemistry, University of Alberta, Alberta T6G 2G2 (Canada); Li Liang, E-mail: liang.li@ualberta.ca [Department of Chemistry, University of Alberta, Alberta T6G 2G2 (Canada); Ling, Yong-Chien, E-mail: ycling@mx.nthu.edu.tw [Department of Chemistry, National Tsing Hua University, Hsinchu 30013, Taiwan (China)

    2012-07-29

    Highlights: Black-Right-Pointing-Pointer MALDI TOFMS is developed as a rapid means of monitoring the process of phthalocyanine derivatives. Black-Right-Pointing-Pointer All-trans retinoic acid is used as matrix to reduce ion fragmentation and background formation. Black-Right-Pointing-Pointer Samples from the reaction process are taken for direct analysis by MALDI TOFMS without any cleanup. Black-Right-Pointing-Pointer The method is demonstrated for monitoring the synthesis of brominated Ni- and Cu-phthalocyanine. - Abstract: Phthalocyanines (PCs), an important class of chemicals widely used in many industrial sectors, are macrocyclic compounds possessing a heteroaromatic {pi}-electron system with optical properties influenced by chemical structures and impurities or by-products introduced during the synthesis process. Analytical tools allowing for rapid monitoring of the synthesis processes are of significance for the development of new PCs with improved performance in many application areas. In this work, we report a matrix-assisted laser desorption/ionization (MALDI) time-of-flight mass spectrometry (TOFMS) method for rapid and convenient monitoring of PC synthesis reactions. For this class of compounds, intact molecular ions could be detected by MALDI using retinoic acid as matrix. It was shown that relative quantification results of two PC compounds could be generated by MALDI MS. This method was applied to monitor the bromination reactions of nickel- and copper-containing PCs. It was demonstrated that, compared to the traditional UV-visible method, the MALDI MS method offers the advantage of higher sensitivity while providing chemical species and relative quantification information on the reactants and products, which are crucial to process monitoring.

  12. Preliminary investigation by liquid chromatography tandem mass spectrometry of perfluorinated compounds presence in bass reared and fished in Italy

    Directory of Open Access Journals (Sweden)

    Federica Farabegoli

    2013-12-01

    Full Text Available The term perfluorinated compounds (PFCs defines synthetic fully-fluorinated compounds; since the 50s they have been largely employed in a wide range of industrial and consumer applications, due to their chemical and physical properties. Only recently, research on their potential adverse effects on both the environment and human health has been conducted, highlighting carcinogenic activity, toxic effects on reproduction, liver and kidney. Human exposure to PFCs is mainly through diet, and in particular fishery products are one of the most contaminated food. Perfluorooctane sulfonate (PFOS and perfluorooctanoic acid (PFOA are the two most important and investigated compounds of this group. The aim of this work was to carry out a preliminary monitoring on the presence of these two molecules in 50 bass muscle samples, of which 30 reared and 20 fished, collected from different Italian areas of the Mediterranean Sea. The method used was based on extraction with organic solvent followed by two purification steps: one with salts and one with dispersive solid phase. The extract was finally analysed by means of an ultra performance liquid chromatographytandem mass spectrometric system. Data showed a relevant contamination of this species and evidenced a significant difference of concentrations between fished (PFOS 112.4- >2000 ng/L and PFOA 3.3-487.0 ng/L and reared basses (PFOS 11.1-104.5 ng/L and PFOA <3-51.4 ng/L. Even if these levels of contamination are sensibly lower than those observed in several studies, fished basses could represent a more relevant source of PFCs exposure in human diet.

  13. Determination of four sulfated vitamin D compounds in human biological fluids by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Gomes, Fabio P; Shaw, P Nicholas; Hewavitharana, Amitha K

    2016-01-15

    The determination of both the water-soluble and lipid-soluble vitamin D compounds in human biological fluids is necessary to illuminate potentially significant biochemical mechanisms. The lack of analytical methods to quantify the water-soluble forms precludes studies on their role and biological functions; currently available liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods are able to determine only a single sulfated form of Vitamin D. We describe here a highly sensitive and specific LC-MS/MS method for the quantification of four sulfated forms of vitamin D: vitamins D2- and D3-sulfate (D2-S and D3-S) and 25-hydroxyvitamin D2- and D3-sulfate (25(OH)D2-S and 25(OH)D3-S). A comparative evaluation showed that the ionization efficiencies of underivatized forms in negative ion mode electrospray ionisation (ESI) are superior to those of the derivatized (using 4-phenyl-l,2,4-triazoline-3,5-dione (PTAD)) forms in positive ion mode ESI. Separation was optimised to minimise co-elution with endogenous matrix compounds, thereby reducing ion suppression/enhancement effects. Isotopically labelled analogues of each compound were used as internal standards to correct for ion suppression/enhancement effects. The method was validated and then applied for the analysis of breastmilk and human serum. The detection limits, repeatability standard deviations, and recoveries ranged from 0.20 to 0.28fmol, 2.8 to 10.2%, and 81.1 to 102%, respectively. PMID:26708628

  14. Simultaneous detection of nonpolar and polar compounds by heat-assisted laser ablation electrospray ionization mass spectrometry.

    Science.gov (United States)

    Vaikkinen, Anu; Shrestha, Bindesh; Nazarian, Javad; Kostiainen, Risto; Vertes, Akos; Kauppila, Tiina J

    2013-01-01

    A heat-assisted laser ablation electrospray ionization (HA-LAESI) method for the simultaneous mass spectrometric analysis of nonpolar and polar analytes was developed. The sample was introduced using mid-infrared laser ablation of a water-rich target. The ablated analytes were ionized with an electrospray plume, which was intercepted by a heated nitrogen gas jet that enhanced the ionization of analytes of low polarity. The feasibility of HA-LAESI was tested by analyzing, e.g., naphtho[2,3-a]pyrene, cholesterol, tricaprylin, 1,1',2,2'-tetramyristoyl cardiolipin, bradykinin fragment 1-8, and 1-palmitoyl-2-oleoyl-sn-glycerol. HA-LAESI was found better suited for low polarity compounds than conventional LAESI, whereas polar compounds were observed with both techniques. The sensitivity of HA-LAESI for the polar bradykinin fragment 1-8 was slightly lower than observed for LAESI. HA-LAESI showed a linear response for 500 nM to 1.0 mM solutions (n = 11) of verapamil with R(2) = 0.988. HA-LAESI was applied for the direct analysis of tissue samples, e.g., avocado (Persea americana) mesocarp and mouse brain tissue sections. Spectra of the avocado showed abundant triglyceride ion peaks, and the results for the mouse brain sections showed cholesterol as the main species. Conventional LAESI shows significantly lower ionization efficiency for these neutral lipids. HA-LAESI can be applied to the analysis of nonpolar and polar analytes, and it extends the capabilities of conventional LAESI to nonpolar and neutral compounds. PMID:23199051

  15. Report on three aliphatic dimethylarsinoyl compounds as common minor constituents in marine samples. An investigation using high-performance liquid chromatography inductively coupled plasma mass spectrometry and electrospray ionisation tandem mass spectrometry

    DEFF Research Database (Denmark)

    Sloth, Jens Jørgen; Larsen, Erik Huusfeldt; Julshamn, K.

    2005-01-01

    chromatography/inductively coupled plasma mass spectrometry (HPLC/ICPMS). Eluate fractions from the HPLC/ICPMS analyses containing the compounds in question were collected and subjected to analysis by electrospray ionisation tandem mass spectrometry (ESI-MS/MS), which provided supportive evidence for the...... of the 37 samples analysed, respectively. The limits of detection were 2-3 mug kg(-1) dry mass. The data illustrate that the three compounds are common minor constituents in marine samples. This is the first report on DMAE and DMAP as naturally occurring species in marine samples. The presence of...

  16. [Determination of volatile organic compounds in ambient air by thermal desorption-gas chromatography-triple quadrupole tandem mass spectrometry].

    Science.gov (United States)

    Feng, Lili; Hu, Xiaofang; Yu, Xiaojuan; Zhang, Wenying

    2016-02-01

    A method was established for the simultaneous determination of 23 volatile organic compounds (VOCs) in ambient air with combination of thermal desorption (TD) and gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS). The air samples were collected by active sampling method using Tenax-TA sorbent tubes, and desorbed by thermal desorption. The analytes were determined by GC-MS/MS in selected reaction monitoring (SRM) mode, and internal standard method was applied to quantify the VOCs. The results of all the 23 VOCs showed good linearities in low level (0. 01-1 ng) and high level (1-100 ng) with all the correlation coefficients (r2) more than 0. 99. The method quantification limits were between 0. 000 08-1 µg/m3. The method was validated by means of recovery experiments (n = 6) at three spiked levels of 2, 10 and 50 ng. The recoveries between 77% and 124% were generally obtained. The relative standard deviations (RSDs) in all cases were lower than 20%, except for chlorobenzene at the low spiked level. The developed method was applied to determine VOCs in ambient air collected at three sites in Shanghai. Several compounds, like benzene, toluene, ethylbenzene, m-xylenes, p-xylenes, styrene, 1, 2, 4-trimethylbenzene and hexachlorobutadiene were detected and confirmed in all the samples analyzed. The method is highly accurate, reliable and sensitive for monitoring the VOCs in ambient air. PMID:27382728

  17. Capillary gas chromatography-ICP mass spectrometry: a powerful hyphenated technique for the determination of organometallic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Smaele, T. de [Laboratory for Analytical Chemistry, Ghent Univ. (Belgium); Moens, L. [Laboratory for Analytical Chemistry, Ghent Univ. (Belgium); Dams, R. [Laboratory for Analytical Chemistry, Ghent Univ. (Belgium); Sandra, P. [Laboratory of Organic Chemistry, Ghent Univ. (Belgium)

    1996-08-01

    The development and improvement of a gas chromatography inductively coupled plasma mass spectrometry system, GC-ICP-MS, is described. The GC and ICP-MS are coupled with a heated stainless steel transfer line. Xe, present in the GC carrier gas, is used to facilitate the nebuliser gas flow rate setting and the positioning of the torch. Alkyltin compounds are separated by GC using a 30 m capillary column within 9 min. The necessity of applying double internal standardisation (use of Bu{sub 3}PeSn and Xe gas as internal standards) is shown. The repeatabilities at 50 {mu}g/l concentration for both retention time and peak are better than 0.25% and 5%, respectively. The detection limits for alkyltin compounds are better than those of existing methods and range between 15 and 35 fg Sn. Finally, GC-ICP-MS is applied to the determination of mono-, di- and tributyltin in some harbour waters, after extraction and Grignard derivation with PrMgCl. Concentrations between 1 and 20 ng/l are found. (orig.). With 5 figs., 6 tabs.

  18. Determination of selected pharmaceutical compounds in biosolids by supported liquid extraction and gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Albero, Beatriz; Sánchez-Brunete, Consuelo; Miguel, Esther; Aznar, Ramón; Tadeo, José L

    2014-04-01

    In this work, an analytical method was developed for the determination of pharmaceutical drugs in biosolids. Samples were extracted with an acidic mixture of water and acetone (1:2, v/v) and supported liquid extraction was used for the clean-up of extracts, eluting with ethyl acetate:methanol (90:10, v/v). The compounds were determined by gas chromatography-tandem mass spectrometry using matrix-match calibration after silylation to form their t-butyldimethylsilyl derivatives. This method presents various advantages, such as a fairly simple operation for the analysis of complex matrices, the use of inexpensive glassware and low solvent volumes. Satisfactory mean recoveries were obtained with the developed method ranging from 70 to 120% with relative standard deviations (RSDs) ≤ 13%, and limits of detection between 0.5 and 3.6 ng g(-1). The method was then successfully applied to biosolids samples collected in Madrid and Catalonia (Spain). Eleven of the sixteen target compounds were detected in the studied samples, at levels up to 1.1 μg g(-1) (salicylic acid). Ibuprofen, caffeine, paracetamol and fenofibrate were detected in all of the samples analyzed. PMID:24582395

  19. Corona discharge ion mobility spectrometry with orthogonal acceleration time of flight mass spectrometry for monitoring of volatile organic compounds.

    Science.gov (United States)

    Sabo, Martin; Matejčík, Štefan

    2012-06-19

    We demonstrate the application of corona discharge ion mobility spectrometry with orthogonal acceleration time of flight mass spectrometry (CD IMS-oaTOF) for volatile organic compounds (VOCs) monitoring. Two-dimensional (2D) IMS-oaTOF spectra of VOCs were recorded in nearly real time. The corona discharge atmospheric pressure chemical ionization (APCI) source was operated in positive mode in nitrogen and air. The CD ion source generates in air H(3)O(+)(H(2)O)(n) and NO(+). The NO(+) offers additional possibility for selective ionization and for an increase of the sensitivity of monoaromatic compounds. In addition to H(3)O(+)(H(2)O)(n) and NO(+), we have carried out ionization of VOCs using acetone as dopant gas ((CH(3))(2)COH(+)). Sixteen model VOCs (tetrahydrofuran, butanol, n-propanol, iso-propano, acetone, methanol, ethanol, toluene, benzene, amomnia, dioxan, triethylamine, acetonitrile, formaldehyde, m-xylene, 2,2,2-trifluoroethylamine) were tested using these ionization techniques. PMID:22594852

  20. Compound nucleus decay along the mass asymmetry coordinate and the role of the Businaro-Gallone point

    International Nuclear Information System (INIS)

    The sharp distinction between evaporation and fission in relatively heavy compound nuclei is a result of a specific topological feature of the liquid drop model potential energy surface V(Z) as a function of mass asymmetry Z. This feature is a deep minimum at symmetry (fission region) flanked at greater asymmetries by the Businaro-Gallone mountains which in turn descend at even larger asymmetries (evaporation region). The experimental cross sections for 530-MeV 74Ge, 782-MeV 93Nb and 1157-MeV 139La + 9Be systems are shown. The cross sections are plotted as a function of charge asymmetry (Z/sub asy/ = Z/sub detected//Z/sub total/). The lack of enhancement in yield near the target Z supports the compound nucleus origin of the products rather than a deep-inelastic origin. The yield from the 74Ge + 9Be system, with a fissility parameter of x = 0.31, decreases steadily as one moves towards symmetry. The yields from the 93Nb + 9Be system (x = 0.40) are essentially constant from Z/sub asy/ = 0.2 to 0.4 while the yields from the 139La + 9Be system (x = 0.50) show the characteristic fission peak at symmetry. These three systems clearly exhibit the qualitative trends expected from the topological changes in the potential energy surface predicted by the liquid drop model

  1. Standard test method for determination of impurities in nuclear grade uranium compounds by inductively coupled plasma mass spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2010-01-01

    1.1 This test method covers the determination of 67 elements in uranium dioxide samples and nuclear grade uranium compounds and solutions without matrix separation by inductively coupled plasma mass spectrometry (ICP-MS). The elements are listed in Table 1. These elements can also be determined in uranyl nitrate hexahydrate (UNH), uranium hexafluoride (UF6), triuranium octoxide (U3O8) and uranium trioxide (UO3) if these compounds are treated and converted to the same uranium concentration solution. 1.2 The elements boron, sodium, silicon, phosphorus, potassium, calcium and iron can be determined using different techniques. The analyst's instrumentation will determine which procedure is chosen for the analysis. 1.3 The test method for technetium-99 is given in Annex A1. 1.4 The values stated in SI units are to be regarded as standard. 1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish ...

  2. Determination of phenolic flame-retardants in human plasma using solid-phase extraction and gas chromatography-electron-capture mass spectrometry.

    Science.gov (United States)

    Thomsen, C; Janák, K; Lundanes, E; Becher, G

    2001-01-01

    A method for determination of phenolic flame-retardants in human plasma utilizing solid-phase extraction (SPE) and gas chromatography with electron-capture mass spectrometric detection (GC-ECMS), has been developed. The plasma lipids were decomposed by application of concentrated sulphuric acid directly on the polystyrene-divinylbenzene SPE column. The method has been validated for 2,4,6-tribromophenol (TriBP), pentabromophenol (PeBP), tetrachlorobisphenol-A (TCBP-A) and tetrabromobisphenol-A (TBBP-A) in the concentration range 1.2-25, 0.4-40, 4-200 and 4-200 pg g(-1) plasma, respectively. The average absolute recovery of the analytes ranged from 51 to 85%. Tetrabromo-o-cresol and chlorotribromobisphenol-A were found suitable as internal standards, and the average recovery of the analytes relative to the internal standards was in the range 93-107%. The repeatability of the method was in the range 4-30% relative standard deviation. The estimated detection limits of TriBP, PeBP, TCBP-A and TBBP-A were 0.3, 0.4, 3.0 and 0.8 pg g(-1) plasma, respectively. The method has been used for analysis of plasma samples from potentially occupationally exposed human individuals. PMID:11204209

  3. Hydrophilic interaction chromatography coupled matrix assisted laser desorption/ionization mass spectrometry for molecular analysis of organic compounds in medicines, tea, and coffee

    KAUST Repository

    Wang, Renqi

    2013-01-01

    Natural occurring organic compounds from food, natural organic matter, as well as metabolic products have received intense attention in current chemical and biological studies. Examination of unknown compounds in complex sample matrices is hampered by the limited choices for data readout and molecular elucidation. Herein, we report a generic method of hydrophilic interaction chromatography (HILIC) coupled with matrix assisted laser desorption/ionization mass spectrometry (MALDI-MS) for the rapid characterization of ingredients in pharmaceutical compounds, tea, and coffee. The analytes were first fractionated using a cationic HILIC column prior to MALDI-MS analyses. It was found that the retention times of a compound arising from different samples were consistent under the same conditions. Accordingly, molecules can be readily characterized by both the mass and chromatographic retention time. The retention behaviors of acidic and basic compounds on the cationic HILIC column were found to be significantly influenced by the pH of mobile phases, whereas neutral compounds depicted a constant retention time at different pH. The general HILIC-MALDI-MS method is feasible for fast screening of naturally occurring organic compounds. A series of homologs can be determined if they have the same retention behavior. Their structural features can be elucidated by considering their mass differences and hydrophilic properties as determined by HILIC chromatogram. © 2013 The Royal Society of Chemistry.

  4. Suitability of magnetic particle immunoassay for the analysis of PBDEs in Hawaiian freshwater fish and crabs in comparison with gas chromatography/electron capture detection-ion trap mass spectrometry

    Science.gov (United States)

    A gas chromatograph/electron capture detector-ion trap mass spectrometer (GC/ECD-ITMS) was used for the determination of polybrominated diphenyl ethers (PBDEs) in freshwater fish and crabs. The samples were also analyzed with an enzyme-linked immunosorbent assay (ELISA). GC/ECD-ITMS results showed...

  5. [Characterization of aroma active compounds in blood orange juice by solid phase microextraction and gas chromatography-mass spectrometry-olfactometry].

    Science.gov (United States)

    Qiao, Yu; Xie, Bijun; Zhang, Yan; Zhang, Yun; Pan, Siyi

    2008-07-01

    Volatile compounds of fresh blood orange juice were analyzed by solid phase microextraction and gas chromatography-mass spectrometry (SPME-GC-MS) and the aroma active compounds were identified by olfactometry. The volatile compounds were extracted by headspace solid phase microextraction (HS-SPME) using a divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber for 40 min at 40 degrees C. The analysis was carried out using an HP 6890N GC equipped with an HP-5 column (30 m x 0.25 mm x 0.25 microm ) directly connected to an HP 5975 series mass selective detector and a sniffing port (ODP2, Gerstel) using helium as carrier gas. Compound identifications were made by the comparison of the mass spectra, retention times, retention indices (I(R)) and odor of the volatile components in the extracts with those of the corresponding reference standards. Forty-six compounds were identified by GC-MS and I(R). The major components of the juice were limonene (86.36%), linalool (3.69%), beta-myrcene (1.79%), octanal (1.32%) and valencene (1.27%). GC-MS-olfactometry analysis was performed to determine 34 compounds with aroma activity, of which 23 compounds were identified. The major contributors to orange juice aroma activity are ethyl butanoate, octanal, gamma-terpinene, 4-acetyl-1-methyleyclohexene, decanal, (-)-carvone, geranyl acetate, valencene. These compounds of strong aroma intensity represent 7.22% of the total volatile compounds. Other four unknown compounds (I(R), <800; I(R) = 1020, 1143, 1169, separately) are also the major contributors to the overall aroma. PMID:18959252

  6. Determining the isotopic abundance of a labeled compound by mass spectrometry and how correcting for natural abundance distribution using analogous data from the unlabeled compound leads to a systematic error.

    Science.gov (United States)

    Schenk, David J; Lockley, William J S; Elmore, Charles S; Hesk, Dave; Roberts, Drew

    2016-04-01

    When the isotopic abundance or specific activity of a labeled compound is determined by mass spectrometry (MS), it is necessary to correct the raw MS data to eliminate ion intensity contributions, which arise from the presence of heavy isotopes at natural abundance (e.g., a typical carbon compound contains ~1.1% (13) C per carbon atom). The most common approach is to employ a correction in which the mass-to-charge distribution of the corresponding unlabeled compound is used to subtract the natural abundance contributions from the raw mass-to-charge distribution pattern of the labeled compound. Following this correction, the residual intensities should be due to the presence of the newly introduced labeled atoms only. However, this will only be the case when the natural abundance mass isotopomer distribution of the unlabeled compound is the same as that of the labeled species. Although this may be a good approximation, it cannot be accurate in all cases. The implications of this approximation for the determination of isotopic abundance and specific activity have been examined in practice. Isotopically mixed stable-atom labeled valine batches were produced, and both these and [(14) C6 ]carbamazepine were analyzed by MS to determine the extent of the error introduced by the approach. Our studies revealed that significant errors are possible for small highly-labeled compounds, such as valine, under some circumstances. In the case with [(14) C6 ]carbamazepine, the errors introduced were minor but could be significant for (14) C-labeled compounds with particular isotopic distributions. This source of systematic error can be minimized, although not eliminated, by the selection of an appropriate isotopic correction pattern or by the use of a program that varies the natural abundance distribution throughout the correction. PMID:26916110

  7. Sample Processing technique onboard ExoMars (MOMA) to analyze organic compounds by Gas Chromatography-Mass Spectrometry

    Science.gov (United States)

    Buch, A.; Freissinet, C.; Sternberg, R.; Szopa, C.; Coll, P. J.; Brault, A.; Pinnick, V.; Siljeström, S.; Raulin, F.; Steininger, H.; Goesmann, F.; MOMA Team

    2011-12-01

    With the aim of separating and detecting organic compounds from Martian soil onboard the Mars Organic Molecule Analyzer (MOMA) experiment of the ExoMars 2018 upcoming joint ESA/NASA mission, we have developed three different space compatible sample preparation techniques compatible with space missions, able to extract and analyze by GC-MS a wide range of volatile and refractory compounds, including chirality analysis. Then, a sample processing utilizing three derivatization/extraction reactions has been carried out. The first reaction is based on a silyl reagent N-Methyl-N- (Tert-Butyldimethylsilyl)trifluoroacetamide (MTBSTFA) [1], the second one, N,N-Dimethylformamide Dimethylacetal (DMF-DMA) [2,3] is dedicated to the chirality detection and the third one is a thermochemolysis based on the use of tetramethylammoniumhydroxide (TMAH). The sample processing system is performed in an oven, dedicated to the MOMA experiment containing the solid sample (50-100mg). The internal temperature of the oven ranges from 20 to 900 °C. The extraction step is achieved by using thermodesorption in the range of 100 to 300°C for 5 to 20 min. Then, the chemical derivatization of the extracted compounds is performed directly on the soil sample by using a derivatyization capsule which contains a mixture of MTBSTFA-DMF or DMF-DMA solution when enantiomeric separation is required. By decreasing the polarity of the targeted molecules, this step allows their volatilization at a temperature below 250°C without any thermal degradation. Once derivatized, the volatile target molecules are trapped in a chemical trap and promptly desorbed into the gas chromatograph coupled to a mass spectrometer. Thermochemolysis is directly performed in the oven at 400°C during 5 min with a 25% (w/w) methanol solution of tetramethylammonium hydroxide (TMAH). Then, pyrolysis in the presence of TMAH allows both an efficient cleavage of polar bonds and the subsequent methylation of COOH, OH and NH2 groups, hence

  8. Alternate strategies to obtain mass balance without the use of radiolabeled compounds: application of quantitative fluorine (19F) nuclear magnetic resonance (NMR) spectroscopy in metabolism studies.

    Science.gov (United States)

    Mutlib, Abdul; Espina, Robert; Atherton, James; Wang, Jianyao; Talaat, Rasmy; Scatina, JoAnn; Chandrasekaran, Appavu

    2012-03-19

    Nuclear magnetic resonance (NMR) spectroscopy is playing an increasingly important role in the quantitation of small and large molecules. Recently, we demonstrated that (1)H NMR could be used to quantitate drug metabolites isolated in submilligram quantities from biological sources. It was shown that these metabolites, once quantitated by NMR, were suitable to be used as reference standards in quantitative LC/MS-based assays, hence circumventing the need for radiolabeled material or synthetic standards to obtain plasma exposure estimates in humans and preclinical species. The quantitative capabilities of high-field NMR is further demonstrated in the current study by obtaining the mass balance of fluorinated compounds using (19)F-NMR. Two fluorinated compounds which were radio-labeled with carbon-14 on metabolically stable positions were dosed in rats and urine and feces collected. The mass balance of the compounds was obtained initially by counting the radioactivity present in each sample. Subsequently, the same sets of samples were analyzed by (19)F-NMR, and the concentrations determined by this method were compared with data obtained using radioactivity counting. It was shown that the two methods produced comparable values. To demonstrate the value of this analytical technique in drug discovery, a fluorinated compound was dosed intravenously in dogs and feces and urine collected. Initial profiling of samples showed that this compound was excreted mainly unchanged in feces, and hence, an estimate of mass balance was obtained using (19)F-NMR. The data obtained by this method was confirmed by additional quantitative studies using mass spectrometry. Hence cross-validations of the quantitative (19)F-NMR method by radioactivity counting and mass spectrometric analysis were demonstrated in this study. A strategy outlining the use of fluorinated compounds in conjunction with (19)F-NMR to understand their routes of excretion or mass balance in animals is proposed. These

  9. The influence of surfactant on mass transfer coefficients in evaporation of volatile organic compound from water basin

    Directory of Open Access Journals (Sweden)

    Bunyakan, C.

    2002-04-01

    Full Text Available Volatile organic compounds (VOCs have been found in wastewater of many chemical industries. Evaporation of VOCs from open water basin in waste treatment facilities causes air-pollution and has been regulated in many countries. Reduction or prevention of VOCs evaporation from open water basin is then necessary. The aim of this research was to investigate the influence of surface film generated by an insoluble surfactant on the mass transfer coefficient of VOCs evaporating from water. Hexadecanol and octadecanol were used as surfactant in this investigation with the amount in the range of 0 to 35 μg/cm2 and 0 to 25 μg/cm2, respectively. The VOCs used in this study were methanol, acetone, methyl ethyl ketone and toluene. The experimental results showed that the surfactant film can reduce the gas film and liquid coefficients by 56 and 80 %, respectively. The suitable amounts of the surfactant were 25 μg/cm2 for hexadecanol and 15 μg/cm2 for octadecanol. From this investigation we can conclude that covering the water surface with a film of hexadecanol or octadecanol could significantly reduce the VOCs evaporation rate.Finally, the empirical equations correlating gas film and liquid film coefficient to amount of surfactants were developed and verified against the experimental data. The predicted values of the overall mass transfer coefficients, obtained by using these empirical equations, were in good agreement with the measured values. Thus the empirical equations of mass transfer coefficients developed in this work can be used to predict the evaporation rates of VOCs from water surface covered by hexadecanol or octadecanol film.

  10. Insights into secondary organic aerosol formed via aqueous-phase reactions of phenolic compounds based on high resolution mass spectrometry

    Directory of Open Access Journals (Sweden)

    Y. Sun

    2010-02-01

    Full Text Available Recent work has shown that aqueous-phase reactions of phenolic compounds – phenol (C6H6O, guaiacol (C7H8O2, and syringol (C8H10O3 – can form secondary organic aerosol (SOA at high yields. Here we examine the chemical characteristics of this SOA and its formation mechanisms using a High-Resolution Time-of-Flight Aerosol Mass Spectrometer (HR-AMS, an Ion Chromatograph (IC, and a Total Organic Carbon (TOC analyzer. The phenolic SOA are highly oxygenated with oxygen-to-carbon (O/C ratios in the range of 0.80–1.06 and carbon oxidation states (=2×O/C–H/C between −0.14 and +0.47. The organic mass-to-carbon (OM/OC ratios determined by the HR-AMS (=2.21���2.55 agree well with values determined based on the SOA mass measured gravimetrically and the OC mass from the TOC analyzer. Both the O/C and OM/OC ratios of the phenolic SOA are similar to the values observed for ambient low-volatility oxygenated/secondary OA (LV-OOA. Oxalate is a minor, but ubiquitous, component of the SOA formed from all three phenolic precursors, accounting for 1.4–5.2% of the SOA mass, with generally higher yields in experiments with H2O2 added as an ·OH source compared to without. The AMS spectra show evidence for the formation of syringol and guaiacol dimers and higher oligomers via C–C and C–O coupling of phenoxyl radicals, which are formed through oxidation pathways such as abstraction of the phenolic hydrogen atom or ·OH addition to the aromatic ring. This latter pathway leads to hydroxylation of the aromatic ring, which is one mechanism that increases the degree of oxidation of the SOA products. Compared to direct photochemical reactions of the phenols, ·OH-initiated reactions favor the formation of smaller oxidation products but less dimers or higher oligomers. Two unique and prominent ions in the syringol and guaiacol SOA spectra,

  11. Luminescent MOFs comprising mixed tritopic linkers and Cd(II)/Zn(II) nodes for selective detection of organic nitro compounds and iodine capture

    Energy Technology Data Exchange (ETDEWEB)

    Rachuri, Yadagiri; Bisht, Kamal Kumar [Analytical Discipline and Centralized Instrument Facility, CSIR–Central Salt and Marine Chemicals Research Institute, Council of Scientific and Industrial Research, G. B. Marg, Bhavnagar 364002, Gujarat (India); Academy of Scientific and Innovative Research (AcSIR), CSIR–Central Salt and Marine Chemicals Research Institute, Council of Scientific and Industrial Research, G. B. Marg, Bhavnagar 364002, Gujarat (India); Parmar, Bhavesh [Analytical Discipline and Centralized Instrument Facility, CSIR–Central Salt and Marine Chemicals Research Institute, Council of Scientific and Industrial Research, G. B. Marg, Bhavnagar 364002, Gujarat (India); Suresh, Eringathodi, E-mail: esuresh@csmcri.org [Analytical Discipline and Centralized Instrument Facility, CSIR–Central Salt and Marine Chemicals Research Institute, Council of Scientific and Industrial Research, G. B. Marg, Bhavnagar 364002, Gujarat (India); Academy of Scientific and Innovative Research (AcSIR), CSIR–Central Salt and Marine Chemicals Research Institute, Council of Scientific and Industrial Research, G. B. Marg, Bhavnagar 364002, Gujarat (India)

    2015-03-15

    Two CPs ([Cd{sub 3}(BTC){sub 2}(TIB){sub 2}(H{sub 2}O){sub 4}].(H{sub 2}O){sub 2}){sub n} (1) and ([Zn{sub 3}(BTC){sub 2}(TIB){sub 2}].(H{sub 2}O){sub 6}){sub n} (2) composed of tripodal linkers BTC (1,3,5-benzenetricarboxylate) and TIB (1,3,5-tris(imidazol-1-ylmethyl)benzene) were synthesized via solvothermal route and structurally characterized. Single crystal structural analysis reveals 1 possesses a novel 3D framework structure, whereas 2 represents a previously established compound. Owing to the d{sup 10} configuration of metal nodes and robust 3D frameworks, 1 and 2 exhibit excellent fluorescence properties which have been exploited to sense organic nitro compounds in vapor phase. Compound 1 demonstrates selective sensing of nitromethane over structurally similar methanol with ca. 70 and 43% fluorescence quenching in case of former and later. Similarly, 58% fluorescence quenching was observed in case of nitrobenzene over the structurally resembling toluene for which 30% quenching was observed. Compound 2 did not show any preference for nitro compounds and exhibited comparable fluorescence quenching when exposed to the vapors of nitro or other geometrically resembling organic molecules. Furthermore, adsorption experiments revealed that 1 and 2 can uptake 2.74 and 14.14 wt% molecular iodine respectively in vapor phase which can be released in organic solvents such as hexane and acetonitrile. The maximal iodine uptake in case of 1 and 2 corresponds to 0.15 and 0.80 molecules of iodine per formula unit of respective frameworks. Comprehensive structural description, thermal stability and luminescence behavior for both CPs has also been presented. - Graphical abstract: Two 3D luminescent CPs comprising mixed tripodal ligands have been hydrothermally synthesized and structurally characterized. Iodine encapsulation capacity of synthesized CPs is evaluated and their fluorescence quenching in presence of small organic molecules is exploited for sensing of nitro

  12. Luminescent MOFs comprising mixed tritopic linkers and Cd(II)/Zn(II) nodes for selective detection of organic nitro compounds and iodine capture

    International Nuclear Information System (INIS)

    Two CPs ([Cd3(BTC)2(TIB)2(H2O)4].(H2O)2)n (1) and ([Zn3(BTC)2(TIB)2].(H2O)6)n (2) composed of tripodal linkers BTC (1,3,5-benzenetricarboxylate) and TIB (1,3,5-tris(imidazol-1-ylmethyl)benzene) were synthesized via solvothermal route and structurally characterized. Single crystal structural analysis reveals 1 possesses a novel 3D framework structure, whereas 2 represents a previously established compound. Owing to the d10 configuration of metal nodes and robust 3D frameworks, 1 and 2 exhibit excellent fluorescence properties which have been exploited to sense organic nitro compounds in vapor phase. Compound 1 demonstrates selective sensing of nitromethane over structurally similar methanol with ca. 70 and 43% fluorescence quenching in case of former and later. Similarly, 58% fluorescence quenching was observed in case of nitrobenzene over the structurally resembling toluene for which 30% quenching was observed. Compound 2 did not show any preference for nitro compounds and exhibited comparable fluorescence quenching when exposed to the vapors of nitro or other geometrically resembling organic molecules. Furthermore, adsorption experiments revealed that 1 and 2 can uptake 2.74 and 14.14 wt% molecular iodine respectively in vapor phase which can be released in organic solvents such as hexane and acetonitrile. The maximal iodine uptake in case of 1 and 2 corresponds to 0.15 and 0.80 molecules of iodine per formula unit of respective frameworks. Comprehensive structural description, thermal stability and luminescence behavior for both CPs has also been presented. - Graphical abstract: Two 3D luminescent CPs comprising mixed tripodal ligands have been hydrothermally synthesized and structurally characterized. Iodine encapsulation capacity of synthesized CPs is evaluated and their fluorescence quenching in presence of small organic molecules is exploited for sensing of nitro organics. - Highlights: • Two 3D mixed ligand coordination polymers containing Cd and Zn center

  13. Applications of Solid-Phase Microextraction and Gas Chromatography/Mass Spectrometry (SPME-GC/MS in the Study of Grape and Wine Volatile Compounds

    Directory of Open Access Journals (Sweden)

    Annarita Panighel

    2014-12-01

    Full Text Available Volatile compounds are responsible for the wine “bouquet”, which is perceived by sniffing the headspace of a glass, and of the aroma component (palate-aroma of the overall flavor, which is perceived on drinking. Grape aroma compounds are transferred to the wine and undergo minimal alteration during fermentation (e.g., monoterpenes and methoxypyrazines; others are precursors of aroma compounds which form in winemaking and during wine aging (e.g., glycosidically-bound volatile compounds and C13-norisoprenoids. Headspace solid phase microextraction (HS-SPME is a fast and simple technique which was developed for analysis of volatile compounds. This review describes some SPME methods coupled with gas chromatography/mass spectrometry (GC/MS used to study the grape and wine volatiles.

  14. Extraction and Characterization of Phenolic Compounds from Rose Hip (Rosa canina L. Using Liquid Chromatography Coupled with Electrospray Ionization - Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Andreea STĂNILĂ

    2015-12-01

    Full Text Available Wild berry are a rich of natural compounds which provide them high antioxidant potential. The compounds which provide them these proprieties are known to be vitamins, flavonoids, anthocyanins and phenolic acids. The aim of this study was to extract and characterize bioactive compounds from rose hip (Rosa canina L. currently found in Romania. A qualitative high-performance liquid chromatography coupled with electrospray ionization mass spectrometric (ESI-MS detection in positive ion mode has been used to identify phenolic compounds from rose hip crude extract. The chromatograms revealed the presence of a large number of compounds (19, identified and grouped as phenolic acids and flavones/ols, flavan-3-ols and also anthocyanins. Based on obtained results these berries can be highly recommended as part of our diet. Also this finding represents a contribution to the chemical characterization of phenolic profile of rose hip.

  15. Structure-dependent degradation of polar compounds in weathered oils observed by atmospheric pressure photo-ionization hydrogen/deuterium exchange ultrahigh resolution mass spectrometry

    International Nuclear Information System (INIS)

    Highlights: • We examined source crude oil and weathered oils from M/V Hebei accident. • APPI hydrogen/deuterium exchange ultrahigh mass spectrometry was applied. • N1 class compounds with 2° and/or 3° amine decrease in larger scale than pyridines. • Preferential degradation of nitrogen-containing compounds was confirmed. • Significant increase in S1O1 compounds was observed as the weathering proceeds. - Abstract: The resin fractions of fresh mixtures of three oils spilled during the M/V Hebei Spirit oil spill, as well as weathered oils collected at weathering stages II and IV from the oil spill site were analyzed and compared by atmospheric pressure photo-ionization hydrogen/deuterium exchange mass spectrometry (HDX MS). The significantly decreased abundance of N+· and [N − H + D]+ ions suggested that secondary and tertiary amine-containing compounds were preferentially degraded during the early stage of weathering. [N + H]+ and [N + D]+ ions previously attributed to pyridine-type compounds degraded more slowly than secondary and tertiary amine-containing compounds. The preferential degradation of nitrogen-containing compounds was confirmed by photo-degradation experiments using 15 standard compounds. In addition, significant increases of [S1O1 + H]+ and [S1O1 + D]+ ions with higher DBE values were observed from fresh oil mixtures as compared to stages II and IV samples, and that could be linked with the decrease of higher DBE compounds of the S1 class. This study presented convincing arguments and evidence demonstrating that secondary and tertiary amines were more vulnerable to photo-degradation than compounds containing pyridine, and hence, preferential degradation depending on chemical structures must be considered in the production of hazardous or toxic components

  16. Structure-dependent degradation of polar compounds in weathered oils observed by atmospheric pressure photo-ionization hydrogen/deuterium exchange ultrahigh resolution mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Islam, Ananna; Kim, Donghwi [Kyungpook National University, Department of Chemistry, Daegu 702-701 (Korea, Republic of); Yim, Un Hyuk; Shim, Won Joon [Oil and POPs Research Group, Korea Institute of Ocean Science and Technology, KIOST, Geoje 656-834 (Korea, Republic of); Kim, Sunghwan, E-mail: sunghwank@knu.ac.kr [Kyungpook National University, Department of Chemistry, Daegu 702-701 (Korea, Republic of); Green Nano Center, Department of Chemistry, Daegu 702-701 (Korea, Republic of)

    2015-10-15

    Highlights: • We examined source crude oil and weathered oils from M/V Hebei accident. • APPI hydrogen/deuterium exchange ultrahigh mass spectrometry was applied. • N{sub 1} class compounds with 2° and/or 3° amine decrease in larger scale than pyridines. • Preferential degradation of nitrogen-containing compounds was confirmed. • Significant increase in S{sub 1}O{sub 1} compounds was observed as the weathering proceeds. - Abstract: The resin fractions of fresh mixtures of three oils spilled during the M/V Hebei Spirit oil spill, as well as weathered oils collected at weathering stages II and IV from the oil spill site were analyzed and compared by atmospheric pressure photo-ionization hydrogen/deuterium exchange mass spectrometry (HDX MS). The significantly decreased abundance of N{sup +}· and [N − H + D]{sup +} ions suggested that secondary and tertiary amine-containing compounds were preferentially degraded during the early stage of weathering. [N + H]{sup +} and [N + D]{sup +} ions previously attributed to pyridine-type compounds degraded more slowly than secondary and tertiary amine-containing compounds. The preferential degradation of nitrogen-containing compounds was confirmed by photo-degradation experiments using 15 standard compounds. In addition, significant increases of [S{sub 1}O{sub 1} + H]{sup +} and [S{sub 1}O{sub 1} + D]{sup +} ions with higher DBE values were observed from fresh oil mixtures as compared to stages II and IV samples, and that could be linked with the decrease of higher DBE compounds of the S{sub 1} class. This study presented convincing arguments and evidence demonstrating that secondary and tertiary amines were more vulnerable to photo-degradation than compounds containing pyridine, and hence, preferential degradation depending on chemical structures must be considered in the production of hazardous or toxic components.

  17. Determination of ginsenoside compound K in human plasma by liquid chromatography–tandem mass spectrometry of lithium adducts

    Directory of Open Access Journals (Sweden)

    Yunhui Chen

    2015-09-01

    Full Text Available Ginsenoside compound K (GCK, the main metabolite of protopanaxadiol constituents of Panax ginseng, easily produces alkali metal adduct ions during mass spectrometry particularly with lithium. Accordingly, we have developed a rapid and sensitive liquid chromatography–tandem mass spectrometric method for analysis of GCK in human plasma based on formation of a lithium adduct. The analyte and paclitaxel (internal standard were extracted from 50 µL human plasma using methyl tert-butyl ether. Chromatographic separation was performed on a Phenomenex Gemini C18 column (50 mm×2.0 mm; 5 μm using stepwise gradient elution with acetonitrile–water and 0.2 mmol/L lithium carbonate at a flow rate of 0.5 mL/min. Detection was performed in the positive ion mode using multiple reaction monitoring of the transitions at m/z 629→449 for the GCK-lithium adduct and m/z 860→292 for the adduct of paclitaxel. The assay was linear in the concentration range 1.00–1000 ng/mL (r2>0.9988 with intra- and inter-day precision of ±8.4% and accuracy in the range of −4.8% to 6.5%. Recovery, stability and matrix effects were all satisfactory. The method was successfully applied to a pharmacokinetic study involving administration of a single GCK 50 mg tablet to healthy Chinese volunteers.

  18. Analysis of volatile organic compounds in Turf by Gas Chromatography-Mass Spectrometry%泥碳中有机挥发物的气相色谱-质谱分析

    Institute of Scientific and Technical Information of China (English)

    王玲; 贾益群; 陈刚

    2004-01-01

    The volatile organic compounds have been separated from the sample in Northeast turf, and these were characterized by gas chromatography-mass spectrometry (GC/MS). 42 compounds were identified using GC/MS library search.

  19. Effective mass enhancement in B site Fe doping heavy fermion compound CaCu3Ru4O12

    Science.gov (United States)

    Wang, Rongjuan; Zhu, Yuanyuan; Wang, Li; Liu, Yong; Shi, Jing; Xiong, Rui

    2015-11-01

    Polycrystalline samples of CaCu3Ru4-xFexO12 (x=0, 0.04, 0.1, 0.2) were synthesized via conventional solid state reactions. The specific heats of these four compounds have been investigated at temperature down to 2 K. Following the Fe doping, the linear electronic specific heat coefficient increased from 90 mJ/(f.u. mol K2) for x=0 to 271 mJ/(f.u. mol) for x=0.2, indicating an effective mass enhancement. We propose that such enhancement mainly comes from the additional Kondo coupling between the itinerant electrons in Ru 4d orbitals and the localized electrons in 3d orbitals of Fe dopants. Moreover, below a certain temperature, an upturn appears in the Cp/T-T2 curves for all the Fe doped samples CaCu3Ru4-xFexO12 with x≤0.2. The origin of this upturn may be a new magnetic order state which needs to be identified with further investigations.

  20. Determination of agrochemical compounds in soya plants by imaging matrix-assisted laser desorption/ionisation mass spectrometry.

    Science.gov (United States)

    Mullen, Alexander K; Clench, Malcolm R; Crosland, Susan; Sharples, Kate R

    2005-01-01

    Detection and imaging of the herbicide mesotrione (2-(4-mesyl-2-nitrobenzoyl)cyclohexane-1,3-dione) and the fungicide azoxystrobin (methyl (E)-2-{2-[6-(2-cyanophenoxy)pyrimidin-4-yloxy]phenyl}-3-methoxyacrylate), on the surface of the soya leaf, and the detection and imaging of azoxystrobin inside the stem of the soya plant, have been achieved using matrix-assisted laser desorption/ionisation quadrupole time-of-flight mass spectrometry. In leaf analysis experiments, the two pesticides were deposited onto the surface of individual soya leaves on growing plants. The soya leaves were removed and prepared for direct and indirect (following blotting onto matrix-coated cellulose membranes) imaging analysis at different periods after initial pesticide application. In stem analysis experiments, azoxystrobin was added to the nutrient solution of a soya plant growing in a hydroponics system. The plant was left for 48 h, and then horizontal and vertical stem sections were prepared for direct imaging analysis. The images obtained demonstrate the applicability of MALDI imaging to the detection and imaging of small organic compounds in plant tissue and further extend the analytical repertoire of the versatile MALDI technique. PMID:16106343

  1. Screening of marine seaweeds for bioactive compound against fish pathogenic bacteria and active fraction analysed by gas chromatography– mass spectrometry

    Directory of Open Access Journals (Sweden)

    Rajasekar Thirunavukkarasu

    2014-05-01

    Full Text Available Objective: To isolate bioactive molecules from marine seaweeds and check the antimicrobial activity against the fish pathogenic bacteria. Methods: Fresh marine seaweeds Gracilaria edulis, Kappaphycus spicifera, Sargassum wightii (S. wightii were collected. Each seaweed was extracted with different solvents. In the study, test pathogens were collected from microbial type culture collection. Antibacterial activity was carried out by using disc diffusion method and minimum inhibition concentration (MIC was calculated. Best seaweed was analysed by fourier transform infrared spectroscopy. The cured extract was separated by thin layer chromatography (TLC. Fraction was collected from TLC to check the antimicrobial activity. Best fraction was analysed by gas chromatography mass spectrometer (GCMS. Results: Based on the disc diffusion method, S. wightii showed a better antimicrobial activity than other seaweed extracts. Based on the MIC, methanol extract of S. wightii showed lower MIC than other solvents. S. wightii were separated by TLC. In this TLC, plate showed a two fraction. These two fractions were separated in preparative TLC and checked for their antimicrobial activity. Fraction 2 showed best MIC value against the tested pathogen. Fraction 2 was analysed by GCMS. Based on the GCMS, fraction 2 contains n-hexadecanoic acid (59.44%. Conclusions: From this present study, it can be concluded that S. wightii was potential sources of bioactive compounds.

  2. Thomas-forbidden particle capture

    OpenAIRE

    Carter, John H.; Lieber, Michael

    2010-01-01

    At high energies, in particle-capture processes between ions and atoms, classical kinematic requirements show that generally double collision Thomas processes dominate. However, for certain mass-ratios these processes are kinematically forbidden. This paper explores the possibility of capture for such processes by triple or higher order collision processes.

  3. Laser capture.

    Science.gov (United States)

    Potter, S Steven; Brunskill, Eric W

    2012-01-01

    This chapter describes detailed methods used for laser capture microdissection (LCM) of discrete subpopulations of cells. Topics covered include preparing tissue blocks, cryostat sectioning, processing slides, performing the LCM, and purification of RNA from LCM samples. Notes describe the fine points of each operation, which can often mean the difference between success and failure. PMID:22639264

  4. Basic research of boron neutron-capture therapy for treatment of pancreatic cancer. Application of neutron radiography for visualization of boron compound on BNCT

    Energy Technology Data Exchange (ETDEWEB)

    Yanagie, Hironobu [Tokyo Univ. (Japan). Inst. of Medical Science

    1997-02-01

    The cytotoxic effects of locally injected {sup 10}B-immunoliposomes (anti-CEA) on human pancreatic carcinoma xenografts in nude mice were evaluated with thermal neutron irradiation. After thermal neutron irradiation of mice injected with {sup 10}B-immunoliposomes, AsPC-1 tumour growth was suppressed relative to controls. Histopathologically, hyalinization and necrosis were found in {sup 10}B-treated tumours, while tumour tissue injected with saline or saline-containing immunoliposomes showed neither destruction nor necrosis. These results suggest that intratumoral injection of boronated immunoliposomes can increase the retention of {sup 10}B atoms by tumour cells, causing tumour growth suppression in vivo upon thermal neutron irradiation. We prepared boronated PEG-binding bovine serum albumin ({sup 10}B-PEG-BSA). {sup 10}B concentrations in AsPC-1, human pancreatic cancer cells (2 x 10{sup 5} /well) obtained 24 hrs after incubation with {sup 10}B-PEG-BSA was 13.01 {+-} 1.74 ppm. The number of {sup 10}B atoms delivered to the tumor cells was calculated to be 7.83 x 10{sup 11} at 24 hrs after incubation with {sup 10}B-PEG-BSA. These data indicated that the {sup 10}B-PEG-BSA could deliver a sufficient amount of {sup 10}B atoms (more than 10{sup 9} atoms/cell) to the tumor cells to induce cytotoxic effects after incubation upon thermal neutron irradiation. Neutron capture autoradiography by using an Imaging Plate (IP-NCR) was performed on AsPC-1 tumor-bearing mouse that had been given an intratumoral injection of {sup 10}B-PEG BSA or {sup 10}B-cationic liposome. We had demonstrated the {sup 10}B-PEG BSA or {sup 10}B-cationic liposome is taken up by AsPC-1 tumor tissue to a much greater extent than by normal tissues. (J.P.N.)

  5. Basic research of boron neutron-capture therapy for treatment of pancreatic cancer. Application of neutron radiography for visualization of boron compound on BNCT

    International Nuclear Information System (INIS)

    The cytotoxic effects of locally injected 10B-immunoliposomes (anti-CEA) on human pancreatic carcinoma xenografts in nude mice were evaluated with thermal neutron irradiation. After thermal neutron irradiation of mice injected with 10B-immunoliposomes, AsPC-1 tumour growth was suppressed relative to controls. Histopathologically, hyalinization and necrosis were found in 10B-treated tumours, while tumour tissue injected with saline or saline-containing immunoliposomes showed neither destruction nor necrosis. These results suggest that intratumoral injection of boronated immunoliposomes can increase the retention of 10B atoms by tumour cells, causing tumour growth suppression in vivo upon thermal neutron irradiation. We prepared boronated PEG-binding bovine serum albumin (10B-PEG-BSA). 10B concentrations in AsPC-1, human pancreatic cancer cells (2 x 105 /well) obtained 24 hrs after incubation with 10B-PEG-BSA was 13.01 ± 1.74 ppm. The number of 10B atoms delivered to the tumor cells was calculated to be 7.83 x 1011 at 24 hrs after incubation with 10B-PEG-BSA. These data indicated that the 10B-PEG-BSA could deliver a sufficient amount of 10B atoms (more than 109 atoms/cell) to the tumor cells to induce cytotoxic effects after incubation upon thermal neutron irradiation. Neutron capture autoradiography by using an Imaging Plate (IP-NCR) was performed on AsPC-1 tumor-bearing mouse that had been given an intratumoral injection of 10B-PEG BSA or 10B-cationic liposome. We had demonstrated the 10B-PEG BSA or 10B-cationic liposome is taken up by AsPC-1 tumor tissue to a much greater extent than by normal tissues. (J.P.N.)

  6. Impact of intra-arterial administration of boron compounds on dose-volume histograms in boron neutron capture therapy for recurrent head-and-neck tumors

    International Nuclear Information System (INIS)

    Purpose: To analyze the dose-volume histogram (DVH) of head-and-neck tumors treated with boron neutron capture therapy (BNCT) and to determine the advantage of the intra-arterial (IA) route over the intravenous (IV) route as a drug delivery system for BNCT. Methods and Materials: Fifteen BNCTs for 12 patients with recurrent head-and-neck tumors were included in the present study. Eight irradiations were done after IV administration of boronophenylalanine and seven after IA administration. The maximal, mean, and minimal doses given to the gross tumor volume were assessed using a BNCT planning system. Results: The results are reported as median values with the interquartile range. In the IA group, the maximal, mean, and minimal dose given to the gross tumor volume was 68.7 Gy-Eq (range, 38.8-79.9), 45.0 Gy-Eq (range, 25.1-51.0), and 13.8 Gy-Eq (range, 4.8-25.3), respectively. In the IV group, the maximal, mean, and minimal dose given to the gross tumor volume was 24.2 Gy-Eq (range, 21.5-29.9), 16.4 Gy-Eq (range, 14.5-20.2), and 7.8 Gy-Eq (range, 6.8-9.5), respectively. Within 1-3 months after BNCT, the responses were assessed. Of the 6 patients in the IV group, 2 had a partial response, 3 no change, and 1 had progressive disease. Of 4 patients in the IA group, 1 achieved a complete response and 3 a partial response. Conclusion: Intra-arterial administration of boronophenylalanine is a promising drug delivery system for head-and-neck BNCT

  7. Determination of off-flavor compounds, 2-methylisoborneol and geosmin, in salmon fillets using stir bar sorptive extraction–thermal desorption coupled with gas chromatography–mass spectrometry

    Science.gov (United States)

    A sensitive and solvent-less method for the determination of musty and earthy off-flavor compounds, 2-methylisoborneol (MIB) and geosmin (GSM), in salmon tissue was developed using stir bar sorptive extraction -thermal desorption coupled with gas chromatography -mass spectrometry (SBSE -TD -GCMS). M...

  8. Use of thermal desorption gas chromatography-olfactometry/mass spectrometry for the comparison of identified and unidentified odor active compounds emitted from building products containing linseed oil

    DEFF Research Database (Denmark)

    Clausen, P. A.; Knudsen, Henrik Nellemose; Larsen, K.;

    2008-01-01

    The emission of odor active volatile organic compounds (VOCs) from a floor oil based on linseed oil, the linseed oil itself and a low-odor linseed oil was investigated by thermal desorption gas chromatography combined with olfactometry and mass spectrometry (TD-GC-O/MS). The oils were applied to...

  9. PhosProtect - a novel and superior compound to tag and protect phospho-groups during mass spectrometry based phospho-proteomics

    DEFF Research Database (Denmark)

    2012-01-01

    Value Proposition The PhosProtect compound alone (developed and tested, IP secured)* • protects phospho-groups during tandem mass spectrometry, thus reducing problematic neutral loss of phosphate. • provides unique phospho-tag by causing isotopic distribution patterns in MS and MS/MS data. The Ph...

  10. Rapid identification of anti-inflammatory compounds from Tongmai Yangxin Pills by liquid chromatography with high-resolution mass spectrometry and chemometric analysis.

    Science.gov (United States)

    Tao, Shan; Huang, Yi; Chen, Zhui; Chen, Yaqi; Wang, Yi; Wang, Yi

    2015-06-01

    We present an integrated approach to rapidly identify anti-inflammatory compounds of TongmaiYangxin Pills (TMYXP), a botanical drug for the treatment of cardiovascular disease. Liquid chromatography coupled with high-resolution mass spectrometry was used to analyze the chemical composition of TMYXP. Eighty compounds of TMYXP including flavonoids, coumarins, iridoid glycosides, saponins, and lignans, were identified unambiguously or tentatively. After the rapid isolation and bioassay, 18 fractions of TMYXP were obtained and their anti-inflammatory activities were evaluated in lipopolysaccharide-stimulated RAW 264.7 macrophages. We performed chemometric analysis to reveal the correlation between the chemical and pharmacological information of the fractions to facilitate the identification of active compounds. To verify the reliability of the proposed method in discovering active components from a complex mixture, activities of seven compounds, which were positively or negatively related to bioactivity according to calculation, were validated in vitro. Results indicated that six active compounds with high R values exerted certain anti-inflammatory effects in a dose-dependent manner with IC50 values of 53.6-204.1 μM. Our findings suggest that the integrated use of identification based on high-resolution mass spectrometry and chemometric methods could rapidly identify active compounds from complex mixture of natural products. PMID:25943824

  11. Analysis of volatile organic compounds in pleural effusions by headspace solid-phase microextraction coupled with cryotrap gas chromatography and mass spectrometry.

    Science.gov (United States)

    Huang, Zhongping; Zhang, Jie; Zhang, Peipei; Wang, Hong; Pan, Zaifa; Wang, Lili

    2016-07-01

    Headspace solid-phase microextraction coupled with cryotrap gas chromatography and mass spectrometry was applied to the analysis of volatile organic compounds in pleural effusions. The highly volatile organic compounds were separated successfully with high sensitivity by the employment of a cryotrap device, with the construction of a cold column head by freezing a segment of metal capillary with liquid nitrogen. A total of 76 volatile organic compounds were identified in 50 pleural effusion samples (20 malignant effusions and 30 benign effusions). Among them, 34 more volatile organic compounds were detected with the retention time less than 8 min, by comparing with the normal headspace solid-phase microextraction coupled with gas chromatography and mass spectrometry method. Furthermore, 24 volatile organic compounds with high occurrence frequency in pleural effusion samples, 18 of which with the retention time less than 8 min, were selected for the comparative analysis. The results of average peak area comparison and box-plot analysis showed that except for cyclohexanone, 2-ethyl-1-hexanol, and tetramethylbenzene, which have been reported as potential cancer biomarkers, cyclohexanol, dichloromethane, ethyl acetate, n-heptane, ethylbenzene, and xylene also had differential expression between malignant and benign effusions. Therefore, the proposed approach was valuable for the comprehensive characterization of volatile organic compounds in pleural effusions. PMID:27159330

  12. Separation and identification of phenolic compounds in Bidens pilosa L. by ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Liang, Xianrui; Xu, Qiao

    2016-05-01

    A validated method based on ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry was established to separate and identify phenolic compounds in Bidens pilosa L. Mass spectrometry experiments were performed both in positive and negative ion modes. A total of 35 compounds were detected, and 26 phenolic compounds were unequivocally identified or tentatively assigned based on retention time, maximum UV absorption, molecular formula, and fragments. The ultra high performance liquid chromatography method was validated and showed good linearity (R(2) ≧ 0.9996) over the test range. The limits of detection and quantification were above 0.072 and 0.162 μg/mL, respectively. The relative standard deviations of intraday and interday precision were below 0.3 and 1.6%, respectively. PMID:27004754

  13. Profiling monoterpenol glycoconjugation in Vitis vinifera L. cv. Muscat of Alexandria using a novel putative compound database approach, high resolution mass spectrometry and collision induced dissociation fragmentation analysis.

    Science.gov (United States)

    Hjelmeland, Anna K; Zweigenbaum, Jerry; Ebeler, Susan E

    2015-08-01

    In this work we present a novel approach for the identification of plant metabolites using ultrahigh performance liquid chromatography coupled to accurate mass time-of-flight mass spectrometry. The workflow involves developing an in-house compound database consisting of exact masses of previously identified as well as putative compounds. The database is used to screen accurate mass spectrometry (MS) data to identify possible compound matches. Subsequent tandem MS data is acquired for possible matches and used for structural elucidation. The methodology is applied to profile monoterpene glycosides in Vitis vinifera cv. Muscat of Alexandria grape berries over three developmental stages. Monoterpenes are a subclass of terpenes, the largest class of plant secondary metabolites, and are found in two major forms in the plant, "bound" to one or more sugar moieties or "free" of said sugar moieties. In the free form, monoterpenes are noted for their fragrance and play important roles in plant defense and as attractants for pollinators. However, glycoconjugation renders these compounds odorless, and it is this form that the plant uses for monoterpene storage. In order to gain insight into monoterpene biochemistry and their fate in the plant an analysis of intact glycosides is essential. Eighteen monoterpene glycosides were identified including a monoterpene trisaccharide glycoside, which is tentatively identified here for this first time in any plant. Additionally, while previous studies have identified monoterpene malonylated glucosides in other grapevine tissue, we tentatively identify them for the first time in grape berries. This analytical approach can be readily applied to other plants and the workflow approach can also be used for other classes of compounds. This approach, in general, provides researchers with data to support the identification of putative compounds, which is especially useful when no standard is available. PMID:26320795

  14. Determination of polybrominated biphenyls in Tasmanian devils (Sarcophilus harrisii) by gas chromatography coupled to electron capture negative ion tandem mass spectrometry or electron ionization high-resolution mass spectrometry.

    Science.gov (United States)

    Vetter, Walter; Recke, Roland von der; Symons, Robert; Pyecroft, Stephen

    2008-12-01

    Two gas chromatography/mass spectrometry (GC/MS) methods for the determination of polybrominated biphenyls (PBBs) by isotope dilution analysis (IDA) using (13)C(12)-PBB 153 in the presence of polybrominated diphenyl ethers (PBDEs) were compared. Recovery of (13)C(12)-PBB 153 which was added to the extracted lipids before sample purification was commenced ranged from 88-117% (mean value 98.2 +/- 8.9%). Nevertheless, IDA analysis of PBBs using (13)C(12)-labelled congeners is limited by the potential co-elution of PBBs with polybrominated diphenyl ethers (PBDEs). The pair PBB 153 and BDE 154 was inspected since M(+) and [M-2Br](+) ions of (13)C(12)-PBB 153 and BDE 154 were only separated by 4 u. Gas chromatography/electron ionization high-resolution mass spectrometry with selected ion monitoring (GC/EI-HRMS-SIM) was suitable when m/z 475.7449 and m/z 477.7429 were used for (13)C(12)-PBB 153 because they are below the monoisotopic peak of the [M-2Br](+) fragment ion of hexaBDEs at m/z 479.7. Gas chromatography/electron capture negative ion tandem mass spectrometry selected reaction monitoring (GC/ECNI-MS/MS-SRM) measurements could be applied because (13)C(12)-PBB 153 and BDE 154 were separated by GC on a 25-m Factor Four CP-Sil 8MS column.Comparative measurements with GC/EI-HRMS-SIM and GC/ECNI-MSMS-SRM were carried out with samples of Tasmanian devils from Tasmania (Australia), an endangered species due to a virus epidemy which has already proved fatal for half of the population. Both techniques verified concentrations of PBB 153 in the range 0.3-11 ng/g lipids with excellent agreement of the levels in all but two samples. The PBB residue pattern demonstrated that PBB pollution originated from the previous discharge with technical hexabromobiphenyl which is dominated by PBB 153. Other congeners such as PBB 132 and PBB 138 were detected in the Tasmanian devils but the proportions relative to PBB 153 were lower than in the technical product. Samples of healthy and

  15. Phenolic Compounds of Pinus brutia Ten.: Chemical Investigation and Quantitative Analysis Using an Ultra-Performance Liquid Chromatography Tandem Mass Spectrometry with Electrospray Ionization Source

    Directory of Open Access Journals (Sweden)

    İbrahim Kıvrak

    2013-08-01

    Full Text Available In this study, phenolic content of Pinus brutia ’s bark was examined using an ultra-performance liquid chromatography tandem mass spectrometry with electrospray ionization source (UPLC-ESI-MS/MS working in multiple reaction monitoring mode. U ltrasonic extraction method with 50% ethanol solution was used for the extraction of bark. The bark of Pinus brutia consisted of 15 compounds: gallic acid, gentisic acid, protocatechuic acid, 4-hydroxy benzoic acid, catechin hydrate, vanillic acid, caffeic acid, vanillin, p-coumaric acid, ferulic acid, myricetin, resveratrol, luteolin, naringenin, kaempferol. Major compound detected was catechin hydrate (28.305 mg 100 g -1 extract. The phenolic compounds of Pinus brutia extract and pycnogenol were compared, and it is shown that both of them consisted of considerable amount of phenolic compounds.

  16. Regiospecific analysis of neutral ether lipids by liquid chromatography/electrospray ionization/single quadrupole mass spectrometry: validation with synthetic compounds

    DEFF Research Database (Denmark)

    Hartvigsen, Karsten; Ravandi, A.; Bukhave, Klaus;

    2001-01-01

    A reversed-phase high-performance liquid chromatography (HPLC) method with on-line electrospray ionization/collision-induced dissociation/mass spectrometry (ESI/CID/MS) is presented for the regiospecific analysis of synthetic reference compounds of neutral ether lipids. The reference compounds were...... are suggested for each neutral ether lipid class. The present study demonstrates that reversed-phase HPLC and positive ion ESI/CID/MS provide direct and unambiguous information about the configuration and identity of molecular species in neutral 1-O-alkyl-sn-glycerol classes....... characterized by chromatographic retention times, full mass spectra, and fragmentation patterns as an aid to clarify the regiospecificity of ether lipids from natural sources. The results clearly show that single quadrupole mass spectroscopic analysis may elucidate the regiospecific structure of neutral ether...

  17. Application of Cassette Ultracentrifugation Using Non-labeled Compounds and Liquid Chromatography-Tandem Mass Spectrometry Analysis for High-Throughput Protein Binding Determination.

    Science.gov (United States)

    Kieltyka, Kasia; McAuliffe, Brian; Cianci, Christopher; Drexler, Dieter M; Shou, Wilson; Zhang, Jun

    2016-03-01

    Membrane-based devices typically used for serum protein binding determination are not fully applicable to highly lipophilic compounds because of nonspecific binding to the device membrane. Ultracentrifugation, however, completely eliminates the issue by using a membrane-free approach, although its wide application has been limited. This lack of utilization is mainly attributed to 2 factors: the high cost in acquiring and handling of radiolabeled compounds and low assay throughput owing to the difficulties in process automation. To overcome these challenges, we report a high-throughput workflow by cassette ultracentrifugation of nonradiolabeled compounds followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. Twenty compounds with diverse physicochemical and protein binding properties were selected for the evaluation of the workflow. To streamline the working process, approaches of matrix balancing for all the samples for LC-MS/MS analysis and determining free fraction without analytical calibration curves were adopted. Both the discrete ultracentrifugation of individual compounds and cassette ultracentrifugation of all the test compounds followed by simultaneous LC-MS/MS analysis exhibited a linear correlation with literature values, demonstrating respectively the validity of the ultracentrifugation process and the cassette approach. The cassette ultracentrifugation using nonradiolabeled compounds followed by LC-MS/MS analysis has greatly facilitated its application for high-throughput protein binding screening in drug discovery. PMID:26886323

  18. Field measurements of biogenic volatile organic compounds in the atmosphere by dynamic solid-phase microextraction and portable gas chromatography-mass spectrometry

    Science.gov (United States)

    Barreira, Luís Miguel Feijó; Parshintsev, Jevgeni; Kärkkäinen, Niina; Hartonen, Kari; Jussila, Matti; Kajos, Maija; Kulmala, Markku; Riekkola, Marja-Liisa

    2015-08-01

    Biogenic volatile organic compounds (BVOCs) participate in many physicochemical processes in the atmosphere. Studies indicate that some of these volatile compounds can be photo-oxidized to non-volatile species that contribute to atmospheric formation and growth of secondary organic aerosols (SOA). In this study, the applicability of dynamic solid-phase microextraction (SPME) for the sampling of atmospheric BVOCs and their oxidation products was tested. These compounds were then analysed via portable gas chromatography-mass spectrometry (GC-MS). The measurements were performed in mid-summer 2013 at the Station for Measuring Ecosystem-Atmosphere Relations, SMEAR II in Hyytiälä, Finland. Numerous classes of compounds were efficiently sampled on PDMS/DVB coated SPME, thermally desorbed and analysed by GC-MS, including monoterpenes, their oxidation products, and amines. Results were analysed against meteorological conditions observed during the sampling campaign and the total amount of monoterpenes obtained by proton-transfer-reaction mass spectrometry (PTR-MS). The comparison of the referred data with obtained results demonstrated the capability of the dynamic SPME method for fast in-situ sampling and analysis of organic gaseous compounds in the atmosphere with minimal analytical steps.

  19. Influence of mass recovery on the performance of a heat pipe type ammonia sorption refrigeration system using CaCl2/activated carbon as compound adsorbent

    International Nuclear Information System (INIS)

    The performance analyses of a sorption refrigeration system with different mass recovery processes are presented, in which compound adsorbent of CaCl2 and activated carbon is used to improve the mass and heat transfer performances of sorption bed. The heating, cooling and heat recovery processes between two sorption beds were performed by multifunction heat pipes without additional power consumption. The experimental Clapeyron diagrams showed that the cycles with mass recovery (MR), with heat and mass recoveries (HMR), and with mass and heat recoveries (MHR), have better thermodynamic performances when compared with the sorption cycle without mass recovery (MR0). The implementary order of mass recovery and heat recovery has strong influence on the efficacy of mass recovery while it has little influence on the efficacy of heat recovery. In sorption cycles with HMR and with MHR, the hot beds can be pre-cooled and cold beds can be pre-heated effectively during the switching process, and heat consumption from external heat source during desorption phase is thereby reduced. Mass recovery can enlarge cycled refrigerant mass due to the transfer of refrigerant gas between two sorption beds during mass recovery process. In comparison with sorption cycle with MR0, sorption cycles with MR, with HMR, and with MHR can generally improve the coefficient of performance (COP) and specific cooling power (SCP) by more than 20% and 16%, respectively. Especially, sorption cycle with MHR has the highest performance among different mass recovery processes due to the fact that MHR has the advantages of MR and HMR, and it can improve the COP by 46.7% when compared with the cycle with MR0

  20. High-resolution mass spectrometric identification and quantification of glucocorticoid compounds in various wastewaters in the Netherlands

    NARCIS (Netherlands)

    M. Schriks; J.A. van Leerdam; S.C. van der Linden; B. van der Burg; A.P. van Wezel; P. de Voogt

    2010-01-01

    In the past two decades much research effort has focused on the occurrence, effects, and risks of estrogenic compounds. However, increasing emissions of new emerging compounds may also affect the action of hormonal pathways other than the estrogenic hormonal axis. Recently, a suite of novel CALUX bi

  1. Intracellular boron localization and uptake in cell cultures using imaging secondary ion mass spectrometry (ion microscopy) for neutron capture therapy for cancer.

    Science.gov (United States)

    Bennett, B D; Zha, X; Gay, I; Morrison, G H

    1992-01-01

    Quantitative ion microscopy of freeze-fractured, freeze-dried cultured cells is a technique for single cell and subcellular elemental analysis. This review describes the technique and its usefulness in determining the uptake and subcellular distribution of the boron from boron neutron capture therapy drugs. PMID:1511239

  2. Identification and quantification of gaseous organic compounds emitted from biomass burning using two-dimensional gas chromatography/time-of-flight mass spectrometry

    Science.gov (United States)

    Hatch, L. E.; Luo, W.; Pankow, J. F.; Yokelson, R. J.; Stockwell, C. E.; Barsanti, K. C.

    2014-09-01

    The current understanding of secondary organic aerosol (SOA) formation within biomass burning (BB) plumes is limited by the incomplete identification and quantification of the non-methane organic compounds (NMOCs) emitted from such fires. Gaseous organic compounds were collected on sorbent cartridges during laboratory burns as part of the fourth Fire Lab at Missoula Experiment (FLAME-4), with analysis by two-dimensional gas chromatography/time-of-flight mass spectrometry (GC × GC / TOFMS). The sensitivity and resolving power of GC × GC / TOFMS allowed the acquisition of the most extensive data set of BB NMOCs to date, with measurements for 722 positively or tentatively identified compounds. Estimated emission factors (EFs) are presented for these compounds for burns of six different vegetative fuels, including conifer branches, grasses, agricultural residue, and peat. The number of compounds detected from individual burns ranged from 129 to 474, and included extensive isomer groups. For example, 38 monoterpene isomers were observed in the emissions from coniferous fuels; the isomeric ratios were found to be consistent with those reported in relevant essential oils, suggesting that the composition of such oils may be very useful when predicting fuel-dependent terpene emissions. Further, eleven sesquiterpenes were detected and tentatively identified, providing the first reported speciation of sesquiterpenes in gas-phase BB emissions. The calculated EFs for all measured compounds are compared and discussed in the context of potential SOA formation.

  3. Identification and quantification of gaseous organic compounds emitted from biomass burning using two-dimensional gas chromatography-time-of-flight mass spectrometry

    Science.gov (United States)

    Hatch, L. E.; Luo, W.; Pankow, J. F.; Yokelson, R. J.; Stockwell, C. E.; Barsanti, K. C.

    2015-02-01

    The current understanding of secondary organic aerosol (SOA) formation within biomass burning (BB) plumes is limited by the incomplete identification and quantification of the non-methane organic compounds (NMOCs) emitted from such fires. Gaseous organic compounds were collected on sorbent cartridges during laboratory burns as part of the fourth Fire Lab at Missoula Experiment (FLAME-4) and analyzed by two-dimensional gas chromatography-time-of-flight mass spectrometry (GC × GC-ToFMS). The sensitivity and resolving power of GC × GC-ToFMS allowed the acquisition of the most extensive data set of BB NMOCs to date, with measurements for 708 positively or tentatively identified compounds. Estimated emission factors (EFs) are presented for these compounds for burns of six different vegetative fuels, including conifer branches, grasses, agricultural residue, and peat. The number of compounds meeting the peak selection criteria ranged from 129 to 474 among individual burns, and included extensive isomer groups. For example, 38 monoterpene isomers were observed in the emissions from coniferous fuels; the isomeric ratios were found to be consistent with those reported in relevant essential oils, suggesting that the composition of such oils may be very useful when predicting fuel-dependent terpene emissions. Further, 11 sesquiterpenes were detected and tentatively identified, providing the first reported speciation of sesquiterpenes in gas-phase BB emissions. The calculated EFs for all measured compounds are compared and discussed in the context of potential SOA formation.

  4. Gas chromatography–mass spectroscopy optimization by computer simulation, application to the analysis of 93 volatile organic compounds in workplace ambient air

    International Nuclear Information System (INIS)

    Graphical abstract: -- Highlights: •Determination of GC thermodynamic retention parameters from only few preliminary experiments. •Simulation of GC separation for any kind of temperature program. •Identification of coelutions and automatic ion selection for MS quantification. •Example of application to two sets of VOC with 16 and 93 compounds. •Such methodology can be easily transposed to any set of volatile compounds. -- Abstract: GC–MS optimization method including both advantages from chromatographic separation and mass spectrometric detection was designed for a set of 93 volatile organic compounds. Only a few experiments were necessary to determine the thermodynamic retention parameters for all compounds on a RTX-VMS column. From these data, computer simulation was used in order to predict the retention times of the compounds in temperature programmed gas chromatography. Then, an automatic selection of ions from the NIST database was performed and compared to the optimum conditions (full separation of VOC). This simulation-selection procedure was used to screen a numerous set of GC and MS conditions in order to quickly design a GC–MS method whatever the set of compounds considered

  5. Identification and quantification of gaseous organic compounds emitted from biomass burning using two-dimensional gas chromatography/time-of-flight mass spectrometry

    Directory of Open Access Journals (Sweden)

    L. E. Hatch

    2014-09-01

    Full Text Available The current understanding of secondary organic aerosol (SOA formation within biomass burning (BB plumes is limited by the incomplete identification and quantification of the non-methane organic compounds (NMOCs emitted from such fires. Gaseous organic compounds were collected on sorbent cartridges during laboratory burns as part of the fourth Fire Lab at Missoula Experiment (FLAME-4, with analysis by two-dimensional gas chromatography/time-of-flight mass spectrometry (GC × GC / TOFMS. The sensitivity and resolving power of GC × GC / TOFMS allowed the acquisition of the most extensive data set of BB NMOCs to date, with measurements for 722 positively or tentatively identified compounds. Estimated emission factors (EFs are presented for these compounds for burns of six different vegetative fuels, including conifer branches, grasses, agricultural residue, and peat. The number of compounds detected from individual burns ranged from 129 to 474, and included extensive isomer groups. For example, 38 monoterpene isomers were observed in the emissions from coniferous fuels; the isomeric ratios were found to be consistent with those reported in relevant essential oils, suggesting that the composition of such oils may be very useful when predicting fuel-dependent terpene emissions. Further, eleven sesquiterpenes were detected and tentatively identified, providing the first reported speciation of sesquiterpenes in gas-phase BB emissions. The calculated EFs for all measured compounds are compared and discussed in the context of potential SOA formation.

  6. A liquid chromatography-atmospheric pressure photoionization tandem mass spectrometric method for the determination of organosulfur compounds in petroleum asphalt cements.

    Science.gov (United States)

    da Silveira, Géssica Domingos; Faccin, Henrique; Claussen, Luis; Goularte, Rayane Bueno; Do Nascimento, Paulo C; Bohrer, Denise; Cravo, Margareth; Leite, Leni F M; de Carvalho, Leandro Machado

    2016-07-29

    We present a sensitive liquid chromatography-atmospheric pressure photoionization tandem mass spectrometric (UHPLC-APPI-MS/MS) method for the determination of selected organosulfur compounds in Brazilian asphalt cements. It was possible to detect 14 organosulfur compounds of different classes where sulfoxides and sulfones presented higher sensibility in ionization than thiophenes and aromatic sulfides. A dopant-assisted APPI method was also tested, however, when chromatographic flow rate was optimized a decrease in signal was observed for all compounds. PAHs were tested and ruled out as possible interfering compounds and the matrix effect of asphalt cements was within an acceptable range for the quantification of organosulfur compounds. The proposed method was found to have satisfactory linearity and accuracy with recoveries between 83.85 and 110.28% for thianaphthene and 3-methylbenzothiophene, respectively. Therefore, the method allowed the characterization of organosulfur compounds in Brazilian asphalt cements and demonstrated changes in the amount quantified in asphaltenic and maltenic fractions after the RTFOT+SUNTEST aging process. PMID:27342135

  7. Characterization of odor-active compounds in cooked meat of farmed obscure puffer (Takifugu obscurus using gas chromatography–mass spectrometry–olfactometry

    Directory of Open Access Journals (Sweden)

    Ning-Ping Tao

    2014-12-01

    Full Text Available The volatile and odor-active compounds in cooked meat of farmed obscure puffer (Takifugu obscurus were analyzed by gas chromatography–mass spectrometry–olfactometry (GC–MS–O. The volatile compounds were extracted by the simultaneous distillation–extraction (SDE method, then separated and identified by GC–MS. Odor-active compounds in the SDE extract were characterized by GC–MS–O. A total of 68 volatile compounds were found, including 23 aldehydes, 10 alcohols, nine ketones, 17 N- or S-containing compounds and aromatics, three acids, three alkanes, and three esters. Of these, 31 odor-active compounds were detected and identified. Trimethylamine (fishy, octanal (grassy, leafy, green, (E-2-octenal (roast, fatty, 1-octen-3-ol (fishy, fatty, mushroom, grassy, 2-ethyl-1-hexanethiol (cooked fish, (E,E-2,4-octadienal (cooked meat, sweet, 2-acetylthiazole (meaty, roast, nutty, sulfur, 2-acetylpyrrole (nutty, walnut, bread were identified as the key odorants in the cooked meat of farmed obscure puffer based on posterior intensity and time-intensity methods.

  8. Characterisation of Phenolic Compounds in South African Plum Fruits (Prunus salicina Lindl. using HPLC Coupled with Diode-Array, Fluorescence, Mass Spectrometry and On-Line Antioxidant Detection

    Directory of Open Access Journals (Sweden)

    Dalene de Beer

    2013-05-01

    Full Text Available Phenolic compounds are abundant secondary metabolites in plums, with potential health benefits believed to be due to their antioxidant activity, amongst others. Phenolic characterisation of South African Prunus salicina Lindl. plums is necessary to fully evaluate their potential health benefits. An HPLC method using diode-array detection (DAD for quantification of phenolic compounds was improved and fluorescence detection (FLD was added for quantification of flavan-3-ols. Validation of the HPLC-DAD-FLD method showed its suitability for quantification of 18 phenolic compounds, including flavan-3-ols using FLD, and phenolic acids, anthocyanins and flavonols using DAD. The method was suitable for characterisation of the phenolic composition of 11 South African plum cultivars and selections, including various types with yellow and red skin and flesh. The method was used in conjunction with mass spectrometry (MS to identify 24 phenolic compounds. Neochlorogenic acid and cyanidin-3-O-glucoside were the major compounds in most of the plums, while cyanidin-3-O-glucoside was absent in Sun Breeze plums with yellow skin and flesh. Post-column on-line coupling of the ABTS•+ scavenging assay with HPLC-DAD enabled qualitative evaluation of the relative contribution of individual phenolic compounds to the antioxidant activity. The flavan-3-ols, neochlorogenic acid and cyanidin-3-O-glucoside displayed the largest antioxidant response peaks.

  9. The prediction of non-compound nucleus fission contribution as a function of the mass number of projectile to induced fission of Pb nucleus

    Directory of Open Access Journals (Sweden)

    S Soheyli

    2013-03-01

    Full Text Available  The recent investigations show that the size and mass number of the target nucleus in the heavy-ion fission reactions are very important for the angular distribution of fission fragments. In this work, we consider the behavior of fission fragment angular anisotropies within the standard saddle-point statistical model for the 168O, 188O, 199F, 2412Mg, 2814Si, 32 16 S+20882Pb fission reaction systems. As a result, a relation is found between the average contribution of non-compound nucleus fission and the mass number of projectile for these systems. It is also obtained that the onset of this contribution is significant for the projectile with the mass number greater than 20, as well as this quantity is an increasing function of the mass number of projectile. Finally, the comparison condition between α, and α BG is modified for these reaction systems.

  10. Inductively coupled plasma-mass spectrometry for elemental analysis and isotope ratio determinations in individual organic compounds separated by gas chromatography

    International Nuclear Information System (INIS)

    A gas chromatograph (GC) with a packed column was interfaced to an inductively coupled plasma-mass spectrometer (ICP-MS) to yield atomic mass spectra from volatile organic compounds. Atomization of injected compounds was nearly complete and independent of molecular structure, so that elemental ratios could be determined. Detection limits were in the range 0.001 to 400 ng s-1, depending on the ionization energy of the element and its abundance in the background spectrum. The relative standard deviation of measured isotope ratios varied from 0.4% for Br (i.e., a ratio close to unity) to 18% for N (a very large ratio). Thus, GC-ICP-MS provides elemental and isotope ratio information that is complementary to the molecular information derived from GC-MS with conventional ionization methods

  11. Inductively coupled plasma-mass spectrometry for elemental analysis and isotope ratio determinations in individual organic compounds separated by gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Chong, N.S.; Houk, R.S.

    1987-01-01

    A gas chromatograph (GC) with a packed column was interfaced to an inductively coupled plasma-mass spectrometer (ICP-MS) to yield atomic mass spectra from volatile organic compounds. Atomization of injected compounds was nearly complete and independent of molecular structure, so that elemental ratios could be determined. Detection limits were in the range 0.001 to 400 ng s/sup -1/, depending on the ionization energy of the element and its abundance in the background spectrum. The relative standard deviation of measured isotope ratios varied from 0.4% for Br (i.e., a ratio close to unity) to 18% for N (a very large ratio). Thus, GC-ICP-MS provides elemental and isotope ratio information that is complementary to the molecular information derived from GC-MS with conventional ionization methods.

  12. Rapid screening and distribution of bioactive compounds in different parts of Berberis petiolaris using direct analysis in real time mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    Awantika Singh; Vikas Bajpai; Mukesh Srivastava; Kamal Ram Arya; Brijesh Kumar

    2015-01-01

    Berberis petiolaris Wall. ex G. Don, an unexplored medicinal plant belonging to the family Berberidaceae, is a large deciduous shrub found in Western Himalaya between 1800-3000 m. Chemical profiling of fruit, leaf, root and stem was done by direct analysis in real time mass spectrometry followed by multivariate analysis for discrimination among the plant parts. The bioactive compounds, including magnoflorine, berberine, jatrorrhizine, thalifendine/berberrubine, demethyleneberberine, reticuline, 8-oxoberberine, N-methyltetrahydroberberine, tetrahydropalmatine, tetrahydroberberine and palmatine, were identified by their exact mass measurement and the corresponding molecular formula of each compound. A comparative study of distribution pattern for all these bioactive alkaloids showed qualitative and quantitative variations in different parts of B. petiolaris. Principal component analysis clearly dis-criminated each part of B. petiolaris plant.

  13. Characterization of volatile organic compounds from human analogue decomposition using thermal desorption coupled to comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry.

    Science.gov (United States)

    Stadler, Sonja; Stefanuto, Pierre-Hugues; Brokl, Michał; Forbes, Shari L; Focant, Jean-François

    2013-01-15

    Complex processes of decomposition produce a variety of chemicals as soft tissues, and their component parts are broken down. Among others, these decomposition byproducts include volatile organic compounds (VOCs) responsible for the odor of decomposition. Human remains detection (HRD) canines utilize this odor signature to locate human remains during police investigations and recovery missions in the event of a mass disaster. Currently, it is unknown what compounds or combinations of compounds are recognized by the HRD canines. Furthermore, a comprehensive decomposition VOC profile remains elusive. This is likely due to difficulties associated with the nontarget analysis of complex samples. In this study, cadaveric VOCs were collected from the decomposition headspace of pig carcasses and were further analyzed using thermal desorption coupled to comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (TD-GC × GC-TOFMS). Along with an advanced data handling methodology, this approach allowed for enhanced characterization of these complex samples. The additional peak capacity of GC × GC, the spectral deconvolution algorithms applied to unskewed mass spectral data, and the use of a robust data mining strategy generated a characteristic profile of decomposition VOCs across the various stages of soft-tissue decomposition. The profile was comprised of numerous chemical families, particularly alcohols, carboxylic acids, aromatics, and sulfides. Characteristic compounds identified in this study, e.g., 1-butanol, 1-octen-3-ol, 2-and 3-methyl butanoic acid, hexanoic acid, octanal, indole, phenol, benzaldehyde, dimethyl disulfide, and trisulfide, are potential target compounds of decomposition odor. This approach will facilitate the comparison of complex odor profiles and produce a comprehensive VOC profile for decomposition. PMID:23215054

  14. Identification of Li-Ion Battery SEI Compounds through (7)Li and (13)C Solid-State MAS NMR Spectroscopy and MALDI-TOF Mass Spectrometry.

    Science.gov (United States)

    Huff, Laura A; Tavassol, Hadi; Esbenshade, Jennifer L; Xing, Wenting; Chiang, Yet-Ming; Gewirth, Andrew A

    2016-01-13

    Solid-state (7)Li and (13)C MAS NMR spectra of cycled graphitic Li-ion anodes demonstrate SEI compound formation upon lithiation that is followed by changes in the SEI upon delithiation. Solid-state (13)C DPMAS NMR shows changes in peaks associated with organic solvent compounds (ethylene carbonate and dimethyl carbonate, EC/DMC) upon electrochemical cycling due to the formation of and subsequent changes in the SEI compounds. Solid-state (13)C NMR spin-lattice (T1) relaxation time measurements of lithiated Li-ion anodes and reference poly(ethylene oxide) (PEO) powders, along with MALDI-TOF mass spectrometry results, indicate that large-molecular-weight polymers are formed in the SEI layers of the discharged anodes. MALDI-TOF MS and NMR spectroscopy results additionally indicate that delithiated anodes exhibit a larger number of SEI products than is found in lithiated anodes. PMID:26653886

  15. Validation of a headspace trap gas chromatography and mass spectrometry method for the quantitative analysis of volatile compounds from degraded rapeseed oil.

    Science.gov (United States)

    Sghaier, Lilia; Cordella, Christophe B Y; Rutledge, Douglas N; Watiez, Mickaël; Breton, Sylvie; Sassiat, Patrick; Thiebaut, Didier; Vial, Jérôme

    2016-05-01

    Due to lipid oxidation, off-flavors, characterized by a fishy odor, are emitted during the heating of rapeseed oil in a fryer and affect the flavor of rapeseed oil even at low concentrations. Thus, there is a need for analytical methods to identify and quantify these products. To study the headspace composition of degraded rapeseed oil, and more specifically the compounds responsible for the fishy odor, a headspace trap gas chromatography with mass spectrometry method was developed and validated. Six volatile compounds formed during the degradation of rapeseed oil were quantified: 1-penten-3-one, (Z)-4-heptenal, hexanal, nonanal, (E,E)-heptadienal, and (E)-2-heptenal. Validation using accuracy profiles allowed us to determine the valid ranges of concentrations for each compound, with acceptance limits of 40% and tolerance limits of 80%. This method was then successfully applied to real samples of degraded oils. PMID:26990911

  16. Development of an automated mass spectrometry system for the quantitative analysis of liver microsomal incubation samples: a tool for rapid screening of new compounds for metabolic stability.

    Science.gov (United States)

    Korfmacher, W A; Palmer, C A; Nardo, C; Dunn-Meynell, K; Grotz, D; Cox, K; Lin, C C; Elicone, C; Liu, C; Duchoslav, E

    1999-01-01

    There is a continuing need for increased throughput in the evaluation of new drug entities in terms of their pharmacokinetic parameters. One useful parameter that can be measured in vitro using liver microsomal preparations is metabolic stability. In this report, we describe an automated system that can be used for unattended quantitative analysis of liver microsomal samples for a series of compounds. This system is based on the Sciex API 150 (single quadrupole) liquid chromatography/mass spectrometry system and utilizes 96-well plate autosampler technology as well as a custom-designed AppleScript which executes the on-line data processing and report generation. It has the capability of analyzing at least 75 compounds per week or 300 compounds per month in an automated fashion. PMID:10353225

  17. Characterization of odor-active compounds of various Chrysanthemum essential oils by gas chromatography-olfactometry, gas chromatography-mass spectrometry and their correlation with sensory attributes.

    Science.gov (United States)

    Xiao, Zuobing; Fan, Binbin; Niu, Yunwei; Wu, Minling; Liu, Junhua; Ma, Shengtao

    2016-01-15

    Volatiles of five kinds of Chrysanthemum essential oils with different manufactures were characterized by descriptive sensory analysis, gas chromatography-olfactometry (GC-O), gas chromatography-mass spectrometry (GC-MS) and statistics analysis. Six sensory attributes (floral, woody, grassy, fruity, sour and minty) were selected to assess Chrysanthemum essential oils. A total of 38 volatile compounds were detected and quantified using standard substances by GC-O and GC-MS. Terpenes constituted the largest chemical group among the volatiles of the essential oils. Then partial least squares regression (PLSR) was used to elucidate the relationship between sensory attributes and aroma compounds. The result showed that α-pinene, β-thujene, α-terpinolen, β-cubebene, caryophyllene, (Z)β-farnesene, (-)-spathulenol, linalool, camphor, camphene, 4-terpineol, Z-citral and 4-isopropyltoluene were typical aroma compounds covaried with characteristic aroma of Chrysanthemum essential oils. PMID:26735711

  18. Phenolic Compounds of Pinus brutia Ten.: Chemical Investigation and Quantitative Analysis Using an Ultra-Performance Liquid Chromatography Tandem Mass Spectrometry with Electrospray Ionization Source

    OpenAIRE

    İbrahim Kıvrak; Şeyda Kıvrak; Mansur Harmandar; Yunus Çetintaş

    2013-01-01

    In this study, phenolic content of Pinus brutia ’s bark was examined using an ultra-performance liquid chromatography tandem mass spectrometry with electrospray ionization source (UPLC-ESI-MS/MS) working in multiple reaction monitoring mode. U ltrasonic extraction method with 50% ethanol solution was used for the extraction of bark. The bark of Pinus brutia consisted of 15 compounds: gallic acid, gentisic acid, protocatechuic acid, 4-hydroxy benzoic acid, catechin hydrate, vanillic acid, caff...

  19. Mass Balance of Fipronil and Total Toxicity of Fipronil-Related Compounds in Process Streams during Conventional Wastewater and Wetland Treatment

    OpenAIRE

    Supowit, Samuel D.; Sadaria, Akash M.; Reyes, Edward J.; Halden, Rolf U.

    2015-01-01

    Attenuation of the pesticide fipronil and its major degradates was determined during conventional wastewater treatment and wetland treatment. Analysis of flow-weighted composite samples by liquid and gas chromatography–tandem mass spectrometry showed fipronil occurrence at 12–31 ng/L in raw sewage, primary effluent, secondary effluent, chlorinated effluent, and wetland effluent. Mean daily loads of total fipronil related compounds in raw sewage and in plant effluent after chlorination were st...

  20. Coumarins as new matrices for matrix-assisted laser-desorption/ionization Fourier transform ion cyclotron resonance mass spectrometric analysis of hydrophobic compounds

    International Nuclear Information System (INIS)

    Highlights: • Coumarins were used as new MALDI matrices. • Coumarins were used for MALDI-FT ICR MS detection of hydrophobic compounds. • DCA had improvement in detection sensitivity, stability, selectivity and reproducibility. • DCA was applied to sterols detection in yeast cells. - Abstract: Hydrophobic compounds with hydroxyl, aldehyde or ketone groups are generally difficult to detect using matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS), because these compounds have low proton affinity and are poorly ionized by MALDI. Herein, coumarins have been used as new matrices for MALDI-MS analysis of a variety of hydrophobic compounds with low ionization efficiency, including steroids, coenzyme Q10, a cyclic lipopeptide and cholesterol oleate. Five coumarins, including coumarin, umbelliferone, esculetin, 7-hydroxycoumarin-3-carboxylic acid (HCA) and 6,7-dihydroxycoumarin-3-carboxylic acid (DCA), were compared with the conventional matrices of 2,5-dihydroxybenzoic acid (DHB) and α-cyano-4-hydroxycinnamic acid (CHCA). Coumarins with hydroxyl or carboxylic acid groups enabled detection. Taking DCA as an example, this matrix proved to be superior to DHB or CHCA in detection sensitivity, stability, spot-to-spot and sample-to-sample reproducibility, and accuracy. DCA increased the stability of the target compounds and decreased the loss of water. The [M + Na]+ peaks were observed for all target compounds by adding NaCl as an additive, and the [M − H2O + H]+ and [M + H]+ peaks decreased. DCA was selected for the identification of sterols in yeast cells, and thirteen sterols were detected by Fourier transform ion cyclotron resonance (FT ICR) mass spectrometry. This work demonstrates the potential of DCA as a new matrix for detection of hydrophobic molecules by MALDI-MS and provides an alternative tool for screening sterols in antifungal research

  1. Coumarins as new matrices for matrix-assisted laser-desorption/ionization Fourier transform ion cyclotron resonance mass spectrometric analysis of hydrophobic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Hang, E-mail: hangwang@sjtu.edu.cn [Instrumental Analysis Center, Shanghai Jiao Tong University, Dongchuan Road 800, Shanghai 200240 (China); Dai, Bona [Instrumental Analysis Center, Shanghai Jiao Tong University, Dongchuan Road 800, Shanghai 200240 (China); Liu, Bin [Key Laboratory of Kidney Disease Pathogenesis and Intervention of Hubei Province, College of Medicine, Hubei Polytechnic University, Huangshi, Hubei 435003 (China); Lu, Han [Department of Anesthesiology, Ruijin Hospital, Shanghai Jiao Tong University School of Medicine (SJTU-SM), 197, Rui Jin Er Road, Shanghai 200025 (China)

    2015-07-02

    Highlights: • Coumarins were used as new MALDI matrices. • Coumarins were used for MALDI-FT ICR MS detection of hydrophobic compounds. • DCA had improvement in detection sensitivity, stability, selectivity and reproducibility. • DCA was applied to sterols detection in yeast cells. - Abstract: Hydrophobic compounds with hydroxyl, aldehyde or ketone groups are generally difficult to detect using matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS), because these compounds have low proton affinity and are poorly ionized by MALDI. Herein, coumarins have been used as new matrices for MALDI-MS analysis of a variety of hydrophobic compounds with low ionization efficiency, including steroids, coenzyme Q10, a cyclic lipopeptide and cholesterol oleate. Five coumarins, including coumarin, umbelliferone, esculetin, 7-hydroxycoumarin-3-carboxylic acid (HCA) and 6,7-dihydroxycoumarin-3-carboxylic acid (DCA), were compared with the conventional matrices of 2,5-dihydroxybenzoic acid (DHB) and α-cyano-4-hydroxycinnamic acid (CHCA). Coumarins with hydroxyl or carboxylic acid groups enabled detection. Taking DCA as an example, this matrix proved to be superior to DHB or CHCA in detection sensitivity, stability, spot-to-spot and sample-to-sample reproducibility, and accuracy. DCA increased the stability of the target compounds and decreased the loss of water. The [M + Na]{sup +} peaks were observed for all target compounds by adding NaCl as an additive, and the [M − H{sub 2}O + H]{sup +} and [M + H]{sup +} peaks decreased. DCA was selected for the identification of sterols in yeast cells, and thirteen sterols were detected by Fourier transform ion cyclotron resonance (FT ICR) mass spectrometry. This work demonstrates the potential of DCA as a new matrix for detection of hydrophobic molecules by MALDI-MS and provides an alternative tool for screening sterols in antifungal research.

  2. Affinity capture of biotinylated proteins at acidic conditions to facilitate hydrogen/deuterium exchange mass spectrometry analysis of multimeric protein complexes

    DEFF Research Database (Denmark)

    Jensen, Pernille Foged; Jørgensen, Thomas J. D.; Koefoed, Klaus; Nygaard, Frank; Sen, Jette Wagtberg

    2013-01-01

    prior to the HDX-MS experiment. However, when studying protein complexes of more than two proteins, immobilization can possibly introduce steric limitations to the interactions. Here, we present a method based on the high affinity biotin-streptavidin interaction that allows selective capture of...... biotinylated proteins even under the extreme conditions for hydrogen/deuterium exchange quenching i.e. pH 2.5 and 0 °C. This biotin-streptavidin capture strategy allows hydrogen/deuterium exchange to occur in proteins in solution and enables characterization of specific proteins in heteromultimeric protein...... complexes without interference of peptides originating from other interaction partners in the complex. The biotin-streptavidin strategy has been successfully implemented in a model system with two recombinant monoclonal antibodies that target nonoverlapping epitopes on the human epidermal growth factor...

  3. Detection of gaseous compounds by needle trap sampling and direct thermal-desorption photoionization mass spectrometry: concept and demonstrative application to breath gas analysis.

    Science.gov (United States)

    Kleeblatt, Juliane; Schubert, Jochen K; Zimmermann, Ralf

    2015-02-01

    A fast detection method to analyze gaseous organic compounds in complex gas mixtures was developed, using a needle trap device (NTD) in conjunction with thermal-desorption photoionization time-of-flight mass spectrometry (TD-PI-TOFMS). The mass spectrometer was coupled via a deactivated fused silica capillary to an injector of a gas chromatograph. In the hot injector, the analytes collected on the NTD were thermally desorbed and directly transferred to the PI-TOFMS ion source. The molecules are softly ionized either by single photon ionization (SPI, 118 nm) or by resonance enhanced multiphoton ionization (REMPI, 266 nm), and the molecular ion signals are detected in the TOF mass analyzer. Analyte desorption and the subsequent PI-TOFMS detection step only lasts ten seconds. The specific selectivity of REMPI (i.e., aromatic compounds) and universal ionization characteristics render PI-MS as a promising detection system. As a first demonstrative application, the alveolar phase breath gas of healthy, nonsmoking subjects was sampled on NTDs. While smaller organic compounds such as acetone, acetaldehyde, isoprene, or cysteamine can be detected in the breath gas with SPI, REMPI depicts the aromatic substances phenol and indole at 266 nm. In the breath gas of a healthy, smoking male subject, several xenobiotic substances such as benzene, toluene, styrene, and ethylbenzene can be found as well. Furthermore, the NTD-REMPI-TOFMS setup was tested for breath gas taken from a mechanically ventilated pig under continuous intravenous propofol (2,6-diisopropylphenol, narcotic drug) infusion. PMID:25517186

  4. Real-time analysis of organic compounds in ship engine aerosol emissions using resonance-enhanced multiphoton ionisation and proton transfer mass spectrometry.

    Science.gov (United States)

    Radischat, Christian; Sippula, Olli; Stengel, Benjamin; Klingbeil, Sophie; Sklorz, Martin; Rabe, Rom; Streibel, Thorsten; Harndorf, Horst; Zimmermann, Ralf

    2015-08-01

    Organic combustion aerosols from a marine medium-speed diesel engine, capable to run on distillate (diesel fuel) and residual fuels (heavy fuel oil), were investigated under various operating conditions and engine parameters. The online chemical characterisation of the organic components was conducted using a resonance-enhanced multiphoton ionisation time-of-flight mass spectrometer (REMPI TOF MS) and a proton transfer reaction-quadrupole mass spectrometer (PTR-QMS). Oxygenated species, alkenes and aromatic hydrocarbons were characterised. Especially the aromatic hydrocarbons and their alkylated derivatives were very prominent in the exhaust of both fuels. Emission factors of known health-hazardous compounds (e.g. mono- and poly-aromatic hydrocarbons) were calculated and found in higher amounts for heavy fuel oil (HFO) at typical engine loadings. Lower engine loads lead in general to increasing emissions for both fuels for almost every compound, e.g. naphthalene emissions varied for diesel fuel exhaust between 0.7 mg/kWh (75 % engine load, late start of injection (SOI)) and 11.8 mg/kWh (10 % engine load, late SOI) and for HFO exhaust between 3.3 and 60.5 mg/kWh, respectively. Both used mass spectrometric techniques showed that they are particularly suitable methods for online monitoring of combustion compounds and very helpful for the characterisation of health-relevant substances. Graphical abstract Three-dimensional REMPI data of organic species in diesel fuel and heavy fuel oil exhaust. PMID:25600686

  5. Analysis of volatile compounds from Siraitia grosvenorii by headspace solid-phase microextraction and gas chromatography-quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Xia, Yi; Zhang, Fang; Wang, Weiyun; Guo, Yinlong

    2015-01-01

    Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-quadrupole time-of-flight mass spectrometry (GC-QTOF MS) has been used in the present study to isolate and identify volatile components from Siraitia grosvenorii, a herbaceous perennial vine used as a natural sweetener and medicine. Compared with the static HS extraction and the different SPME fiber coatings, HS-SPME with divinylbenzene/carboxen/polydimethylsiloxane fiber was preferred to extract the target analytes including aldehyde, alcohol, acid, ester and other compounds. In the identification, a multi-dimensional qualitative analysis approach containing library searching, retention index comparison, accurate mass measurement, the second-stage mass spectrum (MS(2) spectrum) and area normalization was utilized. Finally, a total of 46 compounds were identified from S. grosvenorii. Among them, n-hexadecanoic acid, 5-hydroxymethylfurfural, 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyran-4-one, (Z, Z)-9,12-octadecadienoic acid and (E, E)-2,4-nonadienal were the main volatile components. The results showed that HS-SPME coupled with GC-QTOF MS is efficient for the extraction of polar volatiles from S. grosvenorii and accurate for the identification of volatile compounds in the complicated matrix. PMID:24668041

  6. Investigation of the mass loss of water soluble ionic compounds caused by EDXRF analysis of PM 10 loaded filters

    OpenAIRE

    YATKIN Sinan; GERBOLES Michel

    2012-01-01

    The PM mass loss due to EDXRF analysis of PM 10 loaded filters was investigated in this study. The mass loss was gravimetrically evaluated on collocated filters analyzed both by EDXRF under vacuum condition and by Ion Chromatography. Then, this comparison was repeated with a gaseous mixture of air and Helium (He) instead of evacuating the measurements chamber of the EDXRF spectrometer. It was shown that EDXRF analysis under vacuum medium leads to mass loss of water soluble ions ...

  7. Analysis of sulfur in carbonaceous compounds by laser microprobe mass spectrometry and temperature-programmed oxidative pyrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Zimny, T.; Weber, J.V.; Krier, G.; Schneider, M.; Fixari, B.; Muller, J.F. [IUT, St. Avold (France). Dept. of Chemistry

    1995-08-01

    The laser microprobe coupled with mass spectrometry and the temperature-programmed oxidative pyrolysis technique are used to analyze sulfur in a range of solid carbonaceous samples containing increasing amounts of sulfur (0.54-5.44% by weight). The results of both techniques are analysed by principal component analysis and multiple linear regression to determine significant mass spectral peaks and in order to establish the correlation between thermal analysis data and mass spectral intensities. The results demonstrate the potential of laser microprobe/mass spectrometry as an analytical tool for sulfur determination in solids.

  8. Molecular-level characterization of crude oil compounds combining reversed-phase high-performance liquid chromatography with off-line high-resolution mass spectrometry

    Science.gov (United States)

    Sim, Arum; Cho, Yunju; Kim, Daae; Witt, Matthias; Birdwell, Justin E.; Kim, Byung Ju; Kim, Sunghwan

    2014-01-01

    A reversed-phase separation technique was developed in a previous study (Loegel et al., 2012) and successfully applied to the de-asphalted fraction of crude oil. However, to the best of our knowledge, the molecular-level characterization of oil fractions obtained by reversed-phase high-performance liquid chromatography (HPLC) coupled with high-resolution mass spectrometry (MS) has not yet been reported. A detailed characterization of the oil fractions prepared by reversed-phase HPLC was performed in this study. HPLC fractionation was carried out on conventional crude oil and an oil shale pyrolysate. The analyses of the fractions showed that the carbon number of alkyl chains and the double bond equivalent (DBE) value were the major factors determining elution order. The compounds with larger DBE (presumably more condensed aromatic structures) and smaller carbon number (presumably compounds with short side chains) were eluted earlier but those compounds with lower DBE values (presumably less aromatic structures) and higher carbon number (presumably compounds with longer alkyl chains) eluted later in the chromatograms. This separation behavior is in good agreement with that expected from the principles of reversed-phase separation. The data presented in this study show that reversed-phase chromatography is effective in separating crude oil compounds and can be combined with ultrahigh-resolution MS data to better understand natural oils and oil shale pyrolysates.

  9. Peptidylation for the determination of low-molecular-weight compounds by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry.

    Science.gov (United States)

    Tang, Feng; Cen, Si-Ying; He, Huan; Liu, Yi; Yuan, Bi-Feng; Feng, Yu-Qi

    2016-05-23

    Determination of low-molecular-weight compounds by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) has been a great challenge in the analytical research field. Here we developed a universal peptide-based derivatization (peptidylation) strategy for the sensitive analysis of low-molecular-weight compounds by MALDI-TOF-MS. Upon peptidylation, the molecular weights of target analytes increase, thus avoiding serious matrix ion interference in the low-molecular-weight region in MALDI-TOF-MS. Since peptides typically exhibit good signal response during MALDI-TOF-MS analysis, peptidylation endows high detection sensitivities of low-molecular-weight analytes. As a proof-of-concept, we analyzed low-molecular-weight compounds of aldehydes and thiols by the developed peptidylation strategy. Our results showed that aldehydes and thiols can be readily determined upon peptidylation, thus realizing the sensitive and efficient determination of low-molecular-weight compounds by MALDI-TOF-MS. Moreover, target analytes also can be unambiguously detected in biological samples using the peptidylation strategy. The established peptidylation strategy is a universal strategy and can be extended to the sensitive analysis of various low-molecular-weight compounds by MALDI-TOF-MS, which may be potentially used in areas such as metabolomics. PMID:27109889

  10. Automated probe microdistillation/mass spectrometry for the analysis of high-molecular weight compounds in fossil fuels

    Energy Technology Data Exchange (ETDEWEB)

    Scheppele, S.E.; Grindstaff, Q.G.; Grigsby, R.D.; Chung, K.C.; Hwang, C.S.; Marriott, T.D.; Schronk, L.R.

    1982-08-01

    Automated probe microdistillation/mass spectroscopy is described. The application of computer hardware and the development of computer software eliminate the dilatory nature of acquiring both the temperature and associated mass spectra and reduces the acquired data for processing. The interaction of various hardware components of the system as well as the associated software is described. (DMC)

  11. Complete characterization of posttranslational modification sites in the bovine milk protein PP3 by tandem mass spectrometry with electron capture dissociation as the last stage

    DEFF Research Database (Denmark)

    Kjeldsen, Frank; Haselmann, Kim F; Budnik, Bogdan A;

    2003-01-01

    the PTM site. Chromatographic peak analysis continues until full sequence coverage is obtained, after which the molecular mass is reconstructed and compared with the measured value. An agreement indicates that the PTM characterization was complete. This procedure applied to the bovine milk PP3 protein......A comprehensive approach to protein identification and determination of sites of posttranslational modifications (PTMs) in heavily modified proteins was tested. In this approach, termed "reconstructed molecular mass analysis" (REMMA), the molecular mass distribution of the intact protein is......-sensitivity PTM characterization of biological important proteins, which should speed up the proteomics research....

  12. Direct Capture at Low Energies

    OpenAIRE

    Balogh, W.; Bieber, R.; Oberhummer, H.; Rauscher, T.; Kratz, K.-L.; Mohr, P; Staudt, G.; Sharma, M. M.

    1994-01-01

    The importance of direct capture for (n,$\\gamma$)--reactions on intermediate-- and heavy--mass target nuclei occuring in the s-- and r--process is investigated. It is shown that the direct mechanism is non--negligible for magic and neutron rich target nuclei. For some double magic and neutron rich nuclei in the r--process direct capture is even the dominant reaction mechanism.

  13. Distinguishing of Ile/Leu amino acid residues in the PP3 protein by (hot) electron capture dissociation in Fourier transform ion cyclotron resonance mass spectrometry.

    Science.gov (United States)

    Kjeldsen, Frank; Haselmann, Kim F; Sørensen, Esben S; Zubarev, Roman A

    2003-03-15

    In hot electron capture dissociation (HECD), multiply protonated polypeptides fragment upon capturing approximately 11-eV electrons. The excess of energy upon the primary c, z* cleavage induces secondary fragmentation in z* fragments. The resultant w ions allow one to distinguish between the isomeric Ile and Leu residues. The analytical utility of HECD is evaluated using tryptic peptides from the bovine milk protein PP3 containing totally 135 amino acid residues. Using a formal procedure for Ile/Leu (Xle) residue assignment, the identities of 20 out of 25 Xle residues (80%) were determined. The identity of an additional two residues could be correctly guessed from the absence of the alternative w ions, and only two residues, for which neither expected nor alternative w ions were observed, remained unassigned. Reinspection of conventional ECD spectra also revealed the presence of Xle w ions, although at lower abundances, with 44% of all Xle residues distinguished. Using a dispenser cathode as an electron source, identification of four out of five Xle residues in a 2.7-kDa peptide was possible with one acquisition 2 s long, with identification of all five residues by averaging of five such acquisitions. Unlike the case of high-energy collision-induced dissociation, no d ions were observed in the HECD of tryptic peptides. PMID:12659185

  14. Determination of Wastewater Compounds in Sediment and Soil by Pressurized Solvent Extraction, Solid-Phase Extraction, and Capillary-Column Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Burkhardt, Mark R.; Zaugg, Steven D.; Smith, Steven G.; ReVello, Rhiannon C.

    2006-01-01

    A method for the determination of 61 compounds in environmental sediment and soil samples is described. The method was developed in response to increasing concern over the effects of endocrine-disrupting chemicals in wastewater and wastewater-impacted sediment on aquatic organisms. This method also may be used to evaluate the effects of combined sanitary and storm-sewer overflow on the water and sediment quality of urban streams. Method development focused on the determination of compounds that were chosen on the basis of their endocrine-disrupting potential or toxicity. These compounds include the alkylphenol ethoxylate nonionic surfactants and their degradates, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclic aromatic hydrocarbons, and high-use domestic pesticides. Sediment and soil samples are extracted using a pressurized solvent extraction system. The compounds of interest are extracted from interfering matrix components by high-pressure water/isopropyl alcohol extraction. The compounds were isolated using disposable solid-phase extraction (SPE) cartridges containing chemically modified polystyrene-divinylbenzene resin. The cartridges were dried with nitrogen gas, and then sorbed compounds were eluted with methylene chloride (80 percent)-diethyl ether (20 percent) through Florisil/sodium sulfate SPE cartridge, and then determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-sand samples fortified at 4 to 72 micrograms averaged 76 percent ?13 percent relative standard deviation for all method compounds. Initial method reporting levels for single-component compounds ranged from 50 to 500 micrograms per kilogram. The concentrations of 20 out of 61 compounds initially will be reported as estimated with the 'E' remark code for one of three reasons: (1) unacceptably low-biased recovery (less than 60 percent) or highly variable method performance

  15. Mass Spectrometric Analysis of Exhaled Breath for the Identification of Volatile Organic Compound Biomarkers in Esophageal and Gastric Adenocarcinoma

    Czech Academy of Sciences Publication Activity Database

    Kumar, S.; Huang, J.; Abbassi-Ghadi, N.; Mackanzie, H. A.; Veselkov, K. A.; Hoare, J. M.; Lovat, L. B.; Španěl, Patrik; Smith, D.; Hanna, G. B.

    2015-01-01

    Roč. 262, č. 6 (2015), s. 981-990. ISSN 0003-4932 Institutional support: RVO:61388955 Keywords : breath analysis * esophageal cancer * mass spectrometry Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 8.327, year: 2014

  16. Determination of pharmaceutical compounds in surface- and ground-water samples by solid-phase extraction and high-performance liquid chromatography-electrospray ionization mass spectrometry

    Science.gov (United States)

    Cahill, J.D.; Furlong, E.T.; Burkhardt, M.R.; Kolpin, D.; Anderson, L.G.

    2004-01-01

    Commonly used prescription and over-the-counter pharmaceuticals are possibly present in surface- and ground-water samples at ambient concentrations less than 1 μg/L. In this report, the performance characteristics of a combined solid-phase extraction isolation and high-performance liquid chromatography–electrospray ionization mass spectrometry (HPLC–ESI-MS) analytical procedure for routine determination of the presence and concentration of human-health pharmaceuticals are described. This method was developed and used in a recent national reconnaissance of pharmaceuticals in USA surface waters. The selection of pharmaceuticals evaluated for this method was based on usage estimates, resulting in a method that contains compounds from diverse chemical classes, which presents challenges and compromises when applied as a single routine analysis. The method performed well for the majority of the 22 pharmaceuticals evaluated, with recoveries greater than 60% for 12 pharmaceuticals. The recoveries of angiotensin-converting enzyme inhibitors, a histamine (H2) receptor antagonist, and antihypoglycemic compound classes were less than 50%, but were retained in the method to provide information describing the potential presence of these compounds in environmental samples and to indicate evidence of possible matrix enhancing effects. Long-term recoveries, evaluated from reagent-water fortifications processed over 2 years, were similar to initial method performance. Method detection limits averaged 0.022 μg/L, sufficient for expected ambient concentrations. Compound-dependent matrix effects on HPLC/ESI-MS analysis, including enhancement and suppression of ionization, were observed as a 20–30% increase in measured concentrations for three compounds and greater than 50% increase for two compounds. Changing internal standard and more frequent ESI source maintenance minimized matrix effects. Application of the method in the national survey demonstrates that several

  17. Development of a gas chromatography-mass spectrometry method to monitor in a single run, mono- to triterpenoid compounds distribution in resinous plant materials.

    Science.gov (United States)

    Jemmali, Zaineb; Chartier, Agnes; Elfakir, Claire

    2016-04-22

    A new procedure based on gas chromatography coupled to mass spectrometry (GC-MS) was developed for the simultaneous determination of mono- to triterpenoid compounds in resinous materials. Given the difference of volatility and polarity of the studied compounds some critical steps in this methodology had to be identified and investigated. The recovery of volatile compounds after sample extraction was studied. A recovery range from 30% to 100% from the more volatile monoterpene to the least one was observed. Then the mandatory derivatization step for the analysis of pentacyclic triterpenes bearing hydroxyl and carboxyl groups was optimized. Results showed that derivatization using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and trimethylchlorosilane (TMCS) in pyridine (22:13:65 v/v/v) for 2h at 30°C was the most efficient method of derivatizing all the hydroxyl and carboxylic acid groups contained in the triterpene structures. After choosing the best injection parameters for these compounds, the selectivity of the GC column towards the separation of these terpenoids was investigated using statistical tools (principal component analysis and desirability functions). A separation with a good resolution was achieved on an HP-5ms column using a programmed temperature vaporizing injector (PTV). The method was pre-validated in terms of detection limits (LOD from 100μgL(-1) to 200μgL(-1) depending on the compound), linearity and repeatability using seven compounds representative of mono- and triterpenoid classes. An exhaustive characterization of various types of resins (di-, triterpenic and oleo-gum resins) was achieved. PMID:27018190

  18. Simultaneous quantification of 50 bioactive compounds of the traditional Chinese medicine formula Gegen-Qinlian decoction using ultra-high performance liquid chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Wang, Qi; Song, Wei; Qiao, Xue; Ji, Shuai; Kuang, Yi; Zhang, Zheng-Xiang; Bo, Tao; Guo, De-An; Ye, Min

    2016-07-01

    The quality evaluation of patent drugs derived from traditional Chinese medicine (TCM) compound formulas has been challenging due to their complex chemical composition. In this study, we developed a solution to evaluate the quality of Gegen-Qinlian Decoction (GQD), an ancient four-herb TCM formula for the treatment of diarrhea and diabetes, together with its derived patent drugs by simultaneously quantifying 50 bioactive compounds. The samples were extracted by 100% methanol (for hydrophobic compounds) and 50% methanol in water (for hydrophilic compounds), respectively, and were separated on a Waters Acquity charged surface hybrid C18 column (2.1×100mm, 1.7μm) eluted with gradients of acetonitrile and water containing 0.1% formic acid at a flow rate of 400μL/min. The analytes were determined by ultra-high performance liquid chromatography coupled with tandem mass spectrometry in the selected reaction monitoring mode. The 50 compounds (including acidic and alkaline, hydrophilic and hydrophobic) were well resolved within 14min, and were determined using an internal standard method. The method was fully validated for precision, repeatability, and recovery. The limits of detection were 0.3-10.0ng/mL. Finally, this method was used to analyze 24 batches of GQD samples, including water decoction, pills, tablets, and oral solutions. Principal component analysis indicated significantly varied chemical compositions among these formulations. The tablets and pills contained higher concentrations of Scutellaria and Coptis compounds than the oral solutions, and the water decoction contained abundant glycosides and saponins. Moreover, the contents of flavanones and flavone O-glucuronides varied remarkably. This study provides a feasible solution for the comprehensive quality control of TCM patent drugs. PMID:27262372

  19. GC-MS in the analysis of organic compounds in meteorites. [Gas Chromatography-Mass Spectroscopy approaches

    Science.gov (United States)

    Lawless, J. G.; Romiez, M. P.

    1974-01-01

    The application of an analytical approach combining gas chromatography with mass spectrometry (GC-MS) has shown that the amino acid composition of meteorite extracts is quite complex. A computer was used in the evaluation of the data obtained in the investigations. The computer programs developed have been concerned solely with the mass spectra of amino acids. Specialized programs have been written to determine the number of carbon atoms in an amino acid which is a member of any of three subclasses.

  20. Control of radioactive wastes and coupling of neutron/gamma measurements: use of radiative capture for the correction of matrix effects that penalize the fissile mass measurement by active neutron interrogation

    International Nuclear Information System (INIS)

    In the framework of radioactive waste drums control, difficulties arise in the nondestructive measurement of fissile mass (235U, 239Pu..) by Active Neutron Interrogation (ANI), when dealing with matrices containing materials (Cl, H...) influencing the neutron flux. The idea is to use the neutron capture reaction (n,γ) to determine the matrix composition to adjust the ANI calibration coefficient value. This study, dealing with 118 litres, homogeneous drums of density less than 0,4 and composed of chlorinated and/or hydrogenated materials, leads to build abacus linking the γ ray peak areas to the ANI calibration coefficient. Validation assays of these abacus show a very good agreement between the corrected and true fissile masses for hydrogenated matrices (max. relative standard deviation: 23 %) and quite good for chlorinated and hydrogenated matrices (58 %). The developed correction method improves the measured values. It may be extended to 0,45 density, heterogeneous drums. (author)

  1. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of semivolatile organic compounds in bottom sediment by solvent extraction, gel permeation chromatographic fractionation, and capillary-column gas chromatography/mass spectrometry

    Science.gov (United States)

    Furlong, E.T.; Vaught, D.G.; Merten, L.M.; Foreman, W.T.; Gates, Paul M.

    1996-01-01

    A method for the determination of 79 semivolatile organic compounds (SOCs) and 4 surrogate compounds in soils and bottom sediment is described. The SOCs are extracted from bottom sediment by solvent extraction, followed by partial isolation using high-performance gel permeation chromatography (GPC). The SOCs then are qualitatively identified and quantitative concentrations determined by capillary-column gas chromatography/mass spectrometry (GC/MS). This method also is designed for an optional simultaneous isolation of polychlorinated biphenyls (PCBs) and organochlorine (OC) insecticides, including toxaphene. When OCs and PCBs are determined, an additional alumina- over-silica column chromatography step follows GPC cleanup, and quantitation is by dual capillary- column gas chromatography with electron-capture detection (GC/ECD). Bottom-sediment samples are centrifuged to remove excess water and extracted overnight with dichloromethane. The extract is concentrated, centrifuged, and then filtered through a 0.2-micrometer polytetrafluoro-ethylene syringe filter. Two aliquots of the sample extract then are quantitatively injected onto two polystyrene- divinylbenzene GPC columns connected in series. The SOCs are eluted with dichloromethane, a fraction containing the SOCs is collected, and some coextracted interferences, including elemental sulfur, are separated and discarded. The SOC-containing GPC fraction then is analyzed by GC/MS. When desired, a second aliquot from GPC is further processed for OCs and PCBs by combined alumina-over-silica column chromatography. The two fractions produced in this cleanup then are analyzed by GC/ECD. This report fully describes and is limited to the determination of SOCs by GC/MS.

  2. Multiresidue analysis of endocrine-disrupting compounds and perfluorinated sulfates and carboxylic acids in sediments by ultra-high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Cavaliere, Chiara; Capriotti, Anna Laura; Ferraris, Francesca; Foglia, Patrizia; Samperi, Roberto; Ventura, Salvatore; Laganà, Aldo

    2016-03-18

    A multiresidue analytical method for the determination of 11 perfluorinated compounds and 22 endocrine-disrupting compounds (ECDs) including 13 natural and synthetic estrogens (free and conjugated forms), 2 alkylphenols, 1 plasticiser, 2 UV-filters, 1 antimicrobial, and 2 organophosphorus compounds in sediments has been developed. Ultrasound-assisted extraction followed by solid phase extraction (SPE) with graphitized carbon black (GCB) cartridge as clean-up step were used. The extraction process yield was optimized in terms of solvent composition. Then, a 3(2) experimental design was used to optimize solvent volume and sonication time by response surface methodology, which simplifies the optimization procedure. The final extract was analyzed by ultra-high performance liquid chromatography coupled with tandem mass spectrometry. The optimized sample preparation method is simple and robust, and allows recovery of ECDs belonging to different classes in a complex matrix such as sediment. The use of GCB for SPE allowed to obtain with a single clean-up procedure excellent recoveries ranging between 75 and 110% (relative standard deviation <16%). The developed methodology has been successfully applied to the analysis of ECDs in sediments from different rivers and lakes of the Lazio Region (Italy). These analyses have shown the ubiquitous presence of chloro-substituted organophosphorus flame retardants and bisphenol A, while other analyzed compounds were occasionally found at concentration between the limit of detection and quantification. PMID:26884138

  3. A comprehensive quantification method for eicosanoids and related compounds by using liquid chromatography/mass spectrometry with high speed continuous ionization polarity switching.

    Science.gov (United States)

    Yamada, Masaki; Kita, Yoshihiro; Kohira, Takahiro; Yoshida, Kenji; Hamano, Fumie; Tokuoka, Suzumi M; Shimizu, Takao

    2015-07-15

    Fatty acids and related metabolites, comprising several hundreds of molecular species, are an important target in disease metabolomics, as they are involved in various mammalian pathologies and physiologies. Selected reaction monitoring (SRM) analysis, which is capable of monitoring hundreds of compounds in a single run, has been widely used for comprehensive quantification. However, it is difficult to monitor a large number of compounds with different ionization polarity, as polarity switching requires a sub-second period per cycle in classical mass spectrometers. In the present study, we developed and evaluated a comprehensive quantification method for eicosanoids and related compounds by using LC/MS with high-speed continuous ionization polarity switching. The new method employs a fast (30ms/cycle) continuous ionization polarity switching, and differentiates 137 targets either by chromatography or by SRM transition. Polarity switching did not affect the lower limits of quantification, which ranged similarly from 0.5 to 200pg on column. Lipid extracts from mouse tissues were analyzed by this method, and 65 targets were quantitatively detected in the brain, including 6 compounds analyzed in the positive ion mode. We demonstrated that a fast continuous ionization polarity switching enables the quantification of a wide variety of lipid mediator species without compromising the sensitivity and reliability. PMID:26046978

  4. Assessment of dispersive liquid-liquid microextraction conditions for gas chromatography time-of-flight mass spectrometry identification of organic compounds in honey.

    Science.gov (United States)

    Moniruzzaman, M; Rodríguez, I; Rodríguez-Cabo, T; Cela, R; Sulaiman, S A; Gan, S H

    2014-11-14

    The suitability of the dispersive liquid-liquid microextraction (DLLME) technique for gas chromatography (GC) characterization of minor organic compounds in honey samples is evaluated. Under optimized conditions, samples were pre-treated by liquid-liquid extraction with acetonitrile followed by DLLME using carbon tetrachloride (CCl4, 0.075 mL) as extractant. The yielded settled phase was analyzed by GC using high resolution time-of-flight (TOF) mass spectrometry (MS). The whole sample preparation process is completed in approximately 10 min, with a total consumption of organic solvents below 4 mL, relative standard deviations lower than 12% and with more than 70 organic compounds, displaying linear retention index in the range from 990 to 2900, identified in the obtained extracts. In comparison with HS SPME extraction, higher peak intensities were attained for most volatile and semi-volatile compounds amenable to both extraction techniques. Furthermore, other species such as highly polar and water soluble benzene acids, long chain fatty acids, esters and flavonoids, which are difficult to concentrate by HS SPME, could be identified in DLLME extracts. Some of the compounds identified in DLLME extracts have been proposed as useful for samples classification and/or they are recognized as markers of honeys from certain geographic areas. PMID:25441341

  5. Molecular formula analysis of fragment ions by isotope-selective collision-induced dissociation tandem mass spectrometry of pharmacologically active compounds.

    Science.gov (United States)

    Bianco, Giuliana; Buchicchio, Alessandro; Lelario, Filomena; Cataldi, Tommaso R I

    2014-12-01

    The purpose of this work is to explore the mass fragment characterization of commonly used drugs through a novel approach, which involves isotope-selective tandem mass spectrometry (MS/MS). Collision-induced dissociation (CID) was performed with a low-resolution linear ion trap mass spectrometer in positive electrospray ionization. Three pharmacologically active ingredients, i.e. omeprazole, meloxicam and brinzolamide, selected as model compounds in their own formulation, were investigated as a sodiated adduct [C17 H19 N3 O3 S + Na](+) (omeprazole) and as protonated adducts, [C14 H13 N3 O4 S2  + H](+) and [C12 H21 N3 O5 S3  + H](+) , meloxicam and brinzolamide, respectively. Selecting a narrow window of ±0.5 m/z units, precursor ion fragmentation by CID-MS/MS of isotopologues A + 0, A + 1 and A + 2 was found very useful to confirm the chemical formula of product ions, thus aiding the establishment of characteristic fragmentation pathways of all three examined compounds. The correctness of putative molecular formula of product ions was easily demonstrated by exploiting the isotope peak abundance ratios (i.e. IF+0 /IF+1 and IF+0 /IF+2 ) as simple constraints in low-resolution MS instrumentations. PMID:25476951

  6. Screening and Identifying of Nephrotoxic Compounds in Lithospermum erythrorhizon Using Live-cell Fluorescence Imaging and Liquid Chromatography Coupled with Tandem Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    ZHAO Xiao-ping; JIN Ye-cheng; ZENG Xing; ZHANG Bo-li; ZHANG Yu-feng

    2011-01-01

    In order to identify the potential nephrotoxic compounds in traditional Chinese medicine Lithospermum erythrorhizon,it was separated into serial fractions according to their polarities.An in vitro method was utilized to determine the nephrotoxicity of these fractions with the help of fluorescence image analysis.As a result,the primary fraction A05 and its secondary fractions C06-C09 and C12-C14 were found to have significant toxicity to LLCPK1 cell line,as determined by the survive rate less than 20% after they were treated with these fractions.These potential nephrotoxic fractions were further analyzed by multistage and high resolution mass spectrometry.The main compounds in these fractions were tentatively identified to be acetylshikonin,isobutyrylshikonin,β,β′-dimethylacryloylshikonin,and isovalerylshikonin,which may bring nephrotoxicity.

  7. Determination of carbonyl compounds in beer by derivatisation and headspace solid-phase microextraction in combination with gas chromatography and mass spectrometry.

    Science.gov (United States)

    Saison, Daan; De Schutter, David P; Delvaux, Filip; Delvaux, Freddy R

    2009-06-26

    Headspace solid-phase microextraction (SPME) followed by gas chromatography and mass spectrometry was applied for quantification of 41 chemically diverse carbonyl compounds in beer. Therefore, in-solution derivatisation with o-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine (PFBHA) combined with SPME was optimised for fibre selection, PFBHA concentration, extraction temperature and time and ionic strength. Afterwards, the method was calibrated and validated successfully and extraction efficiency was compared to sampling with on-fibre derivatisation. In-solution derivatisation enabled the detection of several compounds that were poorly extracted with on-fibre derivatisation such as 5-hydroxymethylfurfural, acrolein, hydroxyacetone, acetoin, glyoxal and methylglyoxal. Others, especially (E)-2-nonenal, were extracted better with on-fibre derivatisation. PMID:19450805

  8. Boron neutron capture therapy. What is next?

    International Nuclear Information System (INIS)

    BNCT (Boron Neutron Capture Therapy) will have difficulties establishing itself without efficient and conclusive clinical trials of glioma, without the expansion to other tumors, and without efficient programs for compound development and testing. (author)

  9. Polydopamine-coated magnetic nanoparticles for isolation and enrichment of estrogenic compounds from surface water samples followed by liquid chromatography-tandem mass spectrometry determination.

    Science.gov (United States)

    Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Piovesana, Susy; Samperi, Roberto; Zenezini Chiozzi, Riccardo; Laganà, Aldo

    2016-06-01

    Estrogens, phytoestrogens, and mycoestrogens may enter into the surface waters from different sources, such as effluents of municipal wastewater treatment plants, industrial plants, and animal farms and runoff from agricultural areas. In this work, a multiresidue analytical method for the determination of 17 natural estrogenic compounds, including four steroid estrogens, six mycoestrogens, and seven phytoestrogens, in river water samples has been developed. (Fe3O4)-based magnetic nanoparticles coated by polydopamine (Fe3O4@pDA) were used for dispersive solid-phase extraction, and the final extract was analyzed by ultra-high performance liquid chromatography coupled with tandem mass spectrometry. The Fe3O4 magnetic nanoparticles were prepared by a co-precipitation procedure, coated by pDA, and characterized by scanning electron microscopy, infrared spectroscopy, and elemental analysis. The sample preparation method was optimized in terms of extraction recovery, matrix effect, selectivity, trueness, precision, method limits of detection, and method limits of quantification (MLOQs). For all the 17 analytes, recoveries were >70 % and matrix effects were below 30 % when 25 mL of river water sample was treated with 90 mg of Fe3O4@pDA nanoparticles. Selectivity was tested by spiking river water samples with 50 other compounds (mycotoxins, antibacterials, conjugated hormones, UV filters, alkylphenols, etc.), and only aflatoxins and some benzophenones showed recoveries >60 %. This method proved to be simple and robust and allowed the determination of natural estrogenic compounds belonging to different classes in surface waters with MLOQs ranging between 0.003 and 0.1 μg L(-1). Graphical Abstract Determination of natural estrogenic compounds in water by magnetic solid phase extraction followed by liquid chromatography-tandem mass spectrometry analysis. PMID:27032407

  10. Solid-phase microextraction and gas chromatography-mass spectrometry of volatile compounds from avocado puree after microwave processing.

    Science.gov (United States)

    López, Mercedes G; Guzmán, G R; Dorantes, A L

    2004-05-14

    Microwave processing offers an alternative to blanch fruits and vegetables, since the application of high temperature and short time often results in minimum damage. An experimental design was used to investigate the effect of microwave time, pH, and avocado leaves (independent variables) on avocado flavor (response) using solid-phase microextraction (SPME)-GC-MS. Among the fully characterized flavor volatiles, 19 compounds were derived from lipid oxidation and only 4 from the avocado leaves. The main components derived from lipids were aldehydes, ketones and alcohols. Terpenoids, estragole, and 2-hexenal [E] were volatiles derived from avocado leaves. When leaves were added to fresh and microwaved avocado terpenoids and 2-hexenal [E]/hexanal ratio increased, this behavior was considered to have a positive effect on the sensorial quality of the product. From the statistical analysis of the experimental design, it was possible to determinate that the most important factors influencing the abundance of flavor compounds derived from lipids were microwave time and pH. Maximum values of these compounds were detected at high levels of microwave time and low values of pH. On the other hand, response surface of terpenoids and estragole showed an increment when microwave time and avocado leaf was increased. The region of optimum response was 30 s microwave time, pH 5.5, and 1% of avocado leaf. PMID:15139417

  11. Determination of a wide range of volatile organic compounds in ambient air using multisorbent adsorption/thermal desorption and gas chromatography/mass spectrometry

    Science.gov (United States)

    Pankow, J.F.; Luo, W.; Isabelle, L.M.; Bender, D.A.; Baker, R.J.

    1998-01-01

    Adsorption/thermal desorption with multisorbent air-sampling cartridges was developed for the determination of 87 method analytes including halogenated alkanes, halogenated alkenes, ethers, alcohols, nitriles, esters, ketones, aromatics, a disulfide, and a furan. The volatilities of the compounds ranged from that of dichlorofluoromethane (CFC12) to that of 1,2,3- trichlorobenzene. The eight most volatile compounds were determined using a 1.5-L air sample and a sample cartridge containing 50 mg of Carbotrap B and 280 mg of Carboxen 1000; the remaining 79 compounds were determined using a 5-L air sample and a cartridge containing 180 mg of Carbotrap B and 70 mg of Carboxen 1000. Analysis and detection were by gas chromatography/mass spectrometry. The minimum detectable level (MDL) concentration values ranged from 0.01 parts per billion by volume (ppbv) for chlorobenzene to 0.4 ppbv for bromomethane; most of the MDL values were in the range 0.02-0.06 ppbv. No breakthrough was detected with the prescribed sample volumes. Analyte stability on the cartridges was very good. Excellent recoveries were obtained with independent check standards. Travel spike recoveries ranged from 90 to 110% for 72 of the 87 compounds. The recoveries were less than 70% for bromomethane and chloroethene and for a few compounds such as methyl acetate that are subject to losses by hydrolysis; the lowest travel spike recovery was obtained for bromomethane (62%). Blank values for all compounds were either below detection or very low. Ambient atmospheric sampling was conducted in New Jersey from April to December, 1997. Three sites characterized by low, moderate, and high densities of urbanization/traffic were sampled. The median detected concentrations of the compounds were either similar at all three sites (as with the chlorofluorocarbon compounds) or increased with the density of urbanization/traffic (as with dichloromethane, MTBE, benzene, and toluene). For toluene, the median detected

  12. Body mass index in young school-age children in relation to organochlorine compounds in early life

    DEFF Research Database (Denmark)

    Høyer, B B; Ramlau-Hansen, C H; Henriksen, T B;

    2014-01-01

    OBJECTIVE: To investigate the association between maternal pregnancy and estimated postnatal serum concentrations of the organochlorines 2,2',4,4',5,5'-hexachlorobiphenyl (CB-153) and 1,1-dichloro-2,2-bis(p-chlorophenyl)ethylene (p,p'-DDE) and body mass index (BMI) z-scores in 5- to 9-year......-old children. METHODS: Maternal sera from the INUENDO birth cohort (2002-2004) comprising mother-child pairs (N=1109) from Greenland, Warsaw (Poland), and Kharkiv (Ukraine) were analysed for CB-153 and p,p'-DDE, using gas chromatography-mass-spectrometry, and were grouped into tertiles for statistical analyses...

  13. Speciation of eight arsenic compounds in human urine by high performance liquid chromatography with inductively coupled plasma mass spectrometric detection using antimonate for internal chromatographic standardization

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Pritzl, G.; Hansen, S. H.

    1993-01-01

    Four anionic and four cationic arsenic compounds in urine were separated by anion- and cation-exchange high-performance liquid chromatography and detected by inductively coupled plasma mass spectrometry (ICP-MS) at m/z 75. The species were the anions arsenite, arsenate, monomethylarsonate and...... arsenate in urine but was stable after at least 4-fold dilution of the urine with water. Arsenite was unstable in both urine samples and standard mixtures when diluted with the basic (pH 10.3) mobile phase used for anion chromatography. This could not be prevented by adding ascorbic acid as antioxidant...

  14. Determination of high molecular mass compounds from Amazonian plant's leaves; Determinacao de compostos de massa molecular alta em folhas de plantas da Amazonia

    Energy Technology Data Exchange (ETDEWEB)

    Siqueira, Denilson Soares de; Pereira, Alberto dos Santos; Aquino Neto, Francisco Radler de [Universidade Federal, Rio de Janeiro, RJ (Brazil). Inst. de Quimica]. E-mail: ladetec@iq.gov.br; Cabral, Jose Augusto; Ferreira, Carlos Alberto Cid [Instituto Nacional de Pesquisas da Amazonia (INPA), Manaus, AM (Brazil); Simoneit, Bernd R.T. [Oregon State Univ., Corvallis, OR (United States). College of Oceanic and Atmospheric Sciences. Petroleum and Environmental Geochemistry Group; Elias, Vladimir O. [Analytical Solution, Rio de Janeiro, RJ (Brazil)

    2003-10-01

    The fractions of dichloromethane extracts of leaves from andiroba (Carapa guianensis - Meliaceae), caapi (Banisteriopsis caapi - Malpighiaceae), cocoa (Theobroma cacao - Sterculiaceae), Brazil nut (Bertholletia excelsa - Lecytidaceae), cupuacu (Theobroma grandiflorum - Sterculiaceae), marupa (Simaruba amara - Simaroubaceae) and rubber tree (Hevea brasiliensis - Euphorbiaceae), were analyzed by HT-HRGC and HT-HRGC-MS. Esters of homologous series of fatty acids and long chain alcohols, phytol, amyrines and tocopherols were characterized. The characterization of the compounds was based mainly in mass spectra data and in addition by usual spectrometric data ({sup 1}H and {sup 13}C NMR, IR). (author)

  15. Neutron capture therapy

    International Nuclear Information System (INIS)

    The overall state of the art related with neutron capture therapy(NCT) is surveyed. Since the field related with NCT is very wide, it is not intended to survey all related subjects in depth. The primary objective of this report is to help those working for the installation of a NCT facility and a PGNAA(prompt gamma ray neutron activation analysis) system for the boron analysis understand overall NCT at Hanaro. Therefore, while the parts of reactor neutron source and PGNAA are dealt in detail, other parts are limited to the level necessary to understand related fields. For example, the subject of chemical compound which requires intensive knowledge on chemistry, is not dealt as a separated item. However, the requirement of a compound for NCT, currently available compounds, their characteristics, etc. could be understood through this report. Although the subject of cancer treated by NCT is out of the capability of the author, it is dealt focussing its characteristics related with the success of NCT. Each detailed subject is expected to be dealt more detail by specialists in future. This report would be helpful for the researchers working for the NCT to understand related fields. (author). 128 refs., 3 tabs., 12 figs

  16. Band structure and effective mass calculations for III-V compound semiconductors using hybrid functionals and optimized local potentials

    International Nuclear Information System (INIS)

    The band structures of III-V semiconductors (InP, InAs, InSb, GaAs, and GaSb) are calculated using the HSE06 hybrid functional, GW, and local potentials optimized for the description of band gaps. We show that the inclusion of a quarter of the exact HF exchange allows to predict accurate direct band gaps for InP, InAs, and InSb, i.e., 1.48, 0.42, 0.28 eV, in good agreement with recent experiments, i.e., 1.42, 0.42, 0.24 eV, respectively. The calculated effective masses and Luttinger parameters are also in reasonable agreement with experiment, although a tendency towards underestimation is observed with increasing anion mass. In order to find more efficient methods than hybrid functionals, the modified Becke-Johnson exchange potential is also employed to calculate the effective masses. The agreement of the effective masses with experiment is comparable to the one obtained with the HSE06 hybrid functional. Therefore, this opens a way to model band structures of much large systems than possible using hybrid functionals.

  17. Quantification of Volatile Compounds in the Headspace of Aqueous Liguids Using Selected Ion Flow Tube Mass Spectrometry

    Czech Academy of Sciences Publication Activity Database

    Španěl, Patrik; Diskin, A. M.; Abbott, S. M.; Wang, T.; Smith, D.

    2002-01-01

    Roč. 16, - (2002), s. 2148-2153. ISSN 0951-4198 R&D Projects: GA ČR GA203/00/0632; GA ČR GA203/02/0737 Institutional research plan: CEZ:AV0Z4040901 Keywords : mass spectrometry * SIFT-MS Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.372, year: 2002

  18. HOLMES. The electron capture decay of {sup 163}Ho to measure the electron neutrino mass with sub-eV sensitivity

    Energy Technology Data Exchange (ETDEWEB)

    Alpert, B. [National Institute of Standards and Technology (NIST), Boulder, CO (United States); Balata, M. [INFN, Laboratori Nazionali del Gran Sasso (LNGS), Assergi, AQ (Italy); Bennett, D. [National Institute of Standards and Technology (NIST), Boulder, CO (United States); Biasotti, M. [Universita di Genova, Dipartimento di Fisica, Genoa (Italy); Sezione di Genova, Istituto Nazionale di Fisica Nucleare (INFN), Genoa (Italy); Boragno, C. [Universita di Genova, Dipartimento di Fisica, Genoa (Italy); Sezione di Genova, Istituto Nazionale di Fisica Nucleare (INFN), Genoa (Italy); Brofferio, C. [Universita di Milano-Bicocca, Dipartimento di Fisica, Milan (Italy); Sezione di Milano-Bicocca, Istituto Nazionale di Fisica Nucleare (INFN), Milan (Italy); Ceriale, V. [Universita di Genova, Dipartimento di Fisica, Genoa (Italy); Sezione di Genova, Istituto Nazionale di Fisica Nucleare (INFN), Genoa (Italy); Corsini, D. [Universita di Genova, Dipartimento di Fisica, Genoa (Italy); Sezione di Genova, Istituto Nazionale di Fisica Nucleare (INFN), Genoa (Italy); Day, P.K. [California Institute of Technology (CALTECH), Jet Propulsion Laboratory, Pasadena, CA (United States); De Gerone, M. [Universita di Genova, Dipartimento di Fisica, Genoa (Italy); Sezione di Genova, Istituto Nazionale di Fisica Nucleare (INFN), Genoa (Italy); Dressler, R. [Paul Scherrer Institut (PSI), Villigen (Switzerland); Faverzani, M. [Universita di Milano-Bicocca, Dipartimento di Fisica, Milan (Italy); Sezione di Milano-Bicocca, Istituto Nazionale di Fisica Nucleare (INFN), Milan (Italy); Ferri, E. [Universita di Milano-Bicocca, Dipartimento di Fisica, Milan (Italy); Sezione di Milano-Bicocca, Istituto Nazionale di Fisica Nucleare (INFN), Milan (Italy); Fowler, J. [National Institute of Standards and Technology (NIST), Boulder, CO (United States); Gatti, F. [Universita di Genova, Dipartimento di Fisica, Genoa (Italy); Sezione di Genova, Istituto Nazionale di Fisica Nucleare (INFN), Genoa (Italy); Giachero, A. [Universita di Milano-Bicocca, Dipartimento di Fisica, Milan (Italy); Sezione di Milano-Bicocca, Istituto Nazionale di Fisica Nucleare (INFN), Milan (Italy); Hays-Wehle, J. [National Institute of Standards and Technology (NIST), Boulder, CO (United States); Heinitz, S. [Paul Scherrer Institut (PSI), Villigen (CH); Hilton, G. [National Institute of Standards and Technology (NIST), Boulder, CO (US); Koester, U. [Institut Laue-Langevin (ILL), Grenoble (FR); Lusignoli, M. [Sezione di Roma 1, Istituto Nazionale di Fisica Nucleare (INFN), Rome (IT); Maino, M. [Universita di Milano-Bicocca, Dipartimento di Fisica, Milan (IT); Sezione di Milano-Bicocca, Istituto Nazionale di Fisica Nucleare (INFN), Milan (IT); Mates, J. [National Institute of Standards and Technology (NIST), Boulder, CO (US); Nisi, S. [INFN, Laboratori Nazionali del Gran Sasso (LNGS), Assergi, AQ (IT); Nizzolo, R. [Universita di Milano-Bicocca, Dipartimento di Fisica, Milan (IT); Sezione di Milano-Bicocca, Istituto Nazionale di Fisica Nucleare (INFN), Milan (IT); Nucciotti, A. [Universita di Milano-Bicocca, Dipartimento di Fisica, Milan (IT); Sezione di Milano-Bicocca, Istituto Nazionale di Fisica Nucleare (INFN), Milan (IT); Pessina, G. [Sezione di Milano-Bicocca, Istituto Nazionale di Fisica Nucleare (INFN), Milan (IT); Pizzigoni, G. [Universita di Genova, Dipartimento di Fisica, Genoa (IT); Sezione di Genova, Istituto Nazionale di Fisica Nucleare (INFN), Genoa (IT); Puiu, A. [Universita di Milano-Bicocca, Dipartimento di Fisica, Milan (IT); Sezione di Milano-Bicocca, Istituto Nazionale di Fisica Nucleare (INFN), Milan (IT); Ragazzi, S. [Universita di Milano-Bicocca, Dipartimento di Fisica, Milan (IT); Sezione di Milano-Bicocca, Istituto Nazionale di Fisica Nucleare (INFN), Milan (IT); Reintsema, C. [National Institute of Standards and Technology (NIST), Boulder, CO (US); Gomes, M.R. [University of Lisbon, Multidisciplinary Centre for Astrophysics (CENTRA-IST), Lisbon (PT); Schmidt, D. [National Institute of Standards and Technology (NIST), Boulder, CO (US); Schumann, D. [Paul Scherrer Institut (PSI), Villigen (CH); Sisti, M. [Universita di Milano-Bicocca, Dipartimento di Fisica, Milan (IT); Sezione di Milano-Bicocca, Istituto Nazionale di Fisica Nucleare (INFN), Milan (IT); Swetz, D. [National Institute of Standards and Technology (NIST), Boulder, CO (US); Terranova, F. [Universita di Milano-Bicocca, Dipartimento di Fisica, Milan (IT); Sezione di Milano-Bicocca, Istituto Nazionale di Fisica Nucleare (INFN), Milan (IT); Ullom, J. [National Institute of Standards and Technology (NIST), Boulder, CO (US)

    2015-03-01

    The European Research Council has recently funded HOLMES, a new experiment to directly measure the neutrino mass. HOLMES will perform a calorimetric measurement of the energy released in the decay of {sup 163}Ho. The calorimetric measurement eliminates systematic uncertainties arising from the use of external beta sources, as in experiments with beta spectrometers. This measurement was proposed in 1982 by A. De Rujula and M. Lusignoli, but only recently the detector technological progress allowed to design a sensitive experiment. HOLMES will deploy a large array of low temperature microcalorimeters with implanted {sup 163}Ho nuclei. The resulting mass sensitivity will be as low as 0.4 eV. HOLMES will be an important step forward in the direct neutrino mass measurement with a calorimetric approach as an alternative to spectrometry. It will also establish the potential of this approach to extend the sensitivity down to 0.1 eV. We outline here the project with its technical challenges and perspectives. (orig.)

  19. Alternative CHCA-based matrices for the analysis of low molecular weight compounds by UV-MALDI-tandem mass spectrometry.

    Science.gov (United States)

    Porta, Tiffany; Grivet, Chantal; Knochenmuss, Richard; Varesio, Emmanuel; Hopfgartner, Gérard

    2011-02-01

    Analysis of low molecular weight compounds (LMWC) in complex matrices by vacuum matrix-assisted laser desorption/ionization (MALDI) often suffers from matrix interferences, which can severely degrade limits of quantitation. It is, therefore, useful to have available a range of suitable matrices, which exhibit complementary regions of interference. Two newly synthesized α-cyanocinnamic acid derivatives are reported here; (E)-2-cyano-3-(naphthalen-2-yl)acrylic acid (NpCCA) and (2E)-3-(anthracen-9-yl)-2-cyanoprop-2enoic acid (AnCCA). Along with the commonly used α-cyano-4-hydroxycinnamic acid (CHCA), and the recently developed 4-chloro-α-cyanocinnamic acid (Cl-CCA) matrices, these constitute a chemically similar series of matrices covering a range of molecular weights, and with correspondingly differing ranges of spectral interference. Their performance was compared by measuring the signal-to-noise ratios (S/N) of 47 analytes, mostly pharmaceuticals, with the different matrices using the selected reaction monitoring (SRM) mode on a triple quadrupole instrument equipped with a vacuum MALDI source. AnCCA, NpCCA and Cl-CCA were found to offer better signal-to-noise ratios in SRM mode than CHCA, but Cl-CCA yielded the best results for 60% of the compounds tested. To better understand the relative performance of this matrix series, the proton affinities (PAs) were measured using the kinetic method. Their relative values were: AnCCA > CHCA > NpCCA > Cl-CCA. This ordering is consistent with the performance data. The synthesis of the new matrices is straightforward and they provide (1) tunability of matrix background interfering ions and (2) enhanced analyte response for certain classes of compounds. PMID:21259393

  20. Difference of Electron Capture and Transfer Dissociation Mass Spectrometry on Ni2+-, Cu2+-, and Zn2+-Polyhistidine Complexes in the Absence of Remote Protons

    Science.gov (United States)

    Asakawa, Daiki; De Pauw, Edwin

    2016-07-01

    Electron capture dissociation (ECD) and electron transfer dissociation (ETD) in metal-peptide complexes are dependent on the metal cation in the complex. The divalent transition metals Ni2+, Cu2+, and Zn2+ were used as charge carriers to produce metal-polyhistidine complexes in the absence of remote protons, since these metal cations strongly bind to neutral histidine residues in peptides. In the case of the ECD and ETD of Cu2+-polyhistidine complexes, the metal cation in the complex was reduced and the recombination energy was redistributed throughout the peptide to lead a zwitterionic peptide form having a protonated histidine residue and a deprotonated amide nitrogen. The zwitterion then underwent peptide bond cleavage, producing a and b fragment ions. In contrast, ECD and ETD induced different fragmentation processes in Zn2+-polyhistidine complexes. Although the N-Cα bond in the Zn2+-polyhistidine complex was cleaved by ETD, ECD of Zn2+-polyhistidine induced peptide bond cleavage accompanied with hydrogen atom release. The different fragmentation modes by ECD and ETD originated from the different electronic states of the charge-reduced complexes resulting from these processes. The details of the fragmentation processes were investigated by density functional theory.

  1. Evaluation of the internal temperatures of an 8.6 kDa protein cation exposed to a hot dispenser cathode employed in electron capture dissociation mass spectrometry.

    Science.gov (United States)

    Yim, Yong-Hyeon; Kim, Byungjoo; Ahn, Seonghee; So, Hun-Young; Lee, Sunyoung; Oh, Han Bin

    2006-01-01

    The 'effective' internal temperature of an 8.6 kDa ubiquitin cation was estimated under electron capture dissociation (ECD) conditions, in which a dispenser cathode electron source was mounted just outside an ion cyclotron resonance (ICR) cell, i.e., axially displaced at a distance less than 1 cm from the rear trap plate of the ICR cell. In this ECD configuration, thermal activation of the molecular ions stored in the ICR cell was anticipated since the heated dispenser cathode (T(cathode surface) > 1000 degrees C) emitted a large amount of (both visible and infrared) radiation as well as electrons. An evaluation of the internal temperature of ubiquitin 6+ and 7+ cations was made by comparing our ECD fragmentation patterns with those obtained by McLafferty et al. (J. Am. Chem. Soc. 2002; 124: 6407) as a function of the ion temperature. In McLafferty's configuration, the heating (or thermal activation) effect of their filament source was minimal since the filament was displaced by a distance as far as 70 cm from their ICR cell. A careful comparison reveals that the fragmentation patterns obtained in this work are very similar to those previously measured at T approximately 125 degrees C. In terms of sequence coverage, our ECD configuration provides better results, and in particular without the aid of any other simultaneous activation method, such as thermal heating, infrared multiphoton irradiation, or collisional activation, except for the visible and infrared radiation from the heated cathode. PMID:16715464

  2. A Variety of Activation Methods Employed in 'Activated-Ion' Electron Capture Dissociation Mass Spectrometry: A Test against Bovine Ubiquitin 7+ Ions

    International Nuclear Information System (INIS)

    Fragmentation efficiencies of various 'activated-ion' electron capture dissociation (AI-ECD) methods are compared for a model system of bovine ubiquitin 7+ cations. In AI-ECD studies, sufficient internal energy was given to protein cations prior to ECD application using IR laser radiation, collisions, blackbody radiation, or in-beam collisions, in turn. The added energy was utilized in increasing the population of the precursor ions with less intra-molecular noncovalent bonds or enhancing thermal fluctuations of the protein cations. Removal of noncovalent bonds resulted in extended structures, which are ECD friendly. Under their best conditions, a variety of activation methods showed a similar effectiveness in ECD fragmentation. In terms of the number of fragmented inter-residue bonds, IR laser/blackbody infrared radiation and 'in-beam' activation were almost equally efficient with ∼70% sequence coverage, while collisions were less productive. In particular, 'in-beam' activation showed an excellent effectiveness in characterizing a pre-fractionated single kind of protein species. However, its inherent procedure did not allow for isolation of the protein cations of interest

  3. Determination of steroid hormones and related compounds in filtered and unfiltered water by solid-phase extraction, derivatization, and gas chromatography with tandem mass spectrometry

    Science.gov (United States)

    Foreman, William T.; Gray, James L.; ReVello, Rhiannon C.; Lindley, Chris E.; Losche, Scott A.; Barber, Larry B.

    2012-01-01

    activated -methyl--trimethylsilyl trifluoroacetamide at 65 degrees Celsius for 1 hour to form trimethylsilyl or trimethylsilyl-enol ether derivatives that are more amenable to gas chromatographic separation than the underivatized compounds. Analysis is carried out by gas chromatography with tandem mass spectrometry using calibration standards that are derivatized concurrently with the sample extracts. Analyte concentrations are quantified relative to specific IDS compounds in the sample, which directly compensate for procedural losses (incomplete recovery) in the determined and reported analyte concentrations. Thus, reported analyte concentrations (or analyte recoveries for spiked samples) are corrected based on recovery of the corresponding IDS compound during the quantification process. Recovery for each IDS compound is reported for each sample and represents an absolute recovery in a manner comparable to surrogate recoveries for other organic methods used by the National Water Quality Laboratory. Thus, IDS recoveries provide a useful tool for evaluating sample-specific analytical performance from an absolute mass recovery standpoint. IDS absolute recovery will differ and typically be lower than the corresponding analyte’s method recovery in spiked samples. However, additional correction of reported analyte concentrations is unnecessary and inappropriate because the analyte concentration (or recovery) already is compensated for by the isotope-dilution quantification procedure. Method analytes were spiked at 10 and 100 nanograms per liter (ng/L) for most analytes (10 times greater spike levels were used for bisphenol A and 100 times greater spike levels were used for 3--coprostanol and cholesterol) into the following validation-sample matrices: reagent water, wastewater-affected surface water, a secondary-treated wastewater effluent, and a primary (no biological treatment) wastewater effluent. Overall method recovery for all analytes in these matrices averaged 100

  4. Mass transfer study between soil, atmosphere, groundwater and building in a contaminated area; volatile organic compounds (VOC)

    International Nuclear Information System (INIS)

    A bibliography review led to detail the mechanisms of exchange between phases and transport of volatile organic compounds in the vadose zone, to put in equations their transfer, to set experimental devices and to define relevant tests. The pollutant in question is trichloroethylene, the porous media is a medium sand and the experiments were implemented in column. Once, an analytical method was available to quantify aqueous, gaseous and sorb TCE, predominant transfers mechanisms were quantified separately especially with diffusion experiments through a sand at three different water contents (dry, residual saturation and saturated). Then, these mechanisms have been coupled in a TCE transfer experiment in sand with a hydrostatic water content profile. Each type of test was dimensioned, if it's possible duplicated and interpreted with the multiphasic software Comsol whose flow equation was changed to consider the gravity driven convection. By strictly controlling external factors and boundary conditions, it was possible to carry out transfer experiments reproducible and interpretable with a volatile and reactive compound in a very permeable porous medium. A good reproducibility of experimental results by simulation was achieved with minor changes in basic parameters: report permeability on viscosity, tortuosity (Millington, 1959) and aerodynamics conductivity curve setting parameter (Thomson et al., 1997). This work has resulted in a fine understanding of gas transfers in the vadose zone, especially in the capillarity fringe. (author)

  5. High Sensitivity Analysis of Nanoliter Volumes of Volatile and Nonvolatile Compounds using Matrix Assisted Ionization (MAI) Mass Spectrometry

    Science.gov (United States)

    Hoang, Khoa; Pophristic, Milan; Horan, Andrew J.; Johnston, Murray V.; McEwen, Charles N.

    2016-06-01

    First results are reported using a simple, fast, and reproducible matrix-assisted ionization (MAI) sample introduction method that provides substantial improvements relative to previously published MAI methods. The sensitivity of the new MAI methods, which requires no laser, high voltage, or nebulizing gas, is comparable to those reported for MALDI-TOF and n-ESI. High resolution full acquisition mass spectra having low chemical background are acquired from low nanoliters of solution using only a few femtomoles of analyte. The limit-of-detection for angiotensin II is less than 50 amol on an Orbitrap Exactive mass spectrometer. Analysis of peptides, including a bovine serum albumin digest, and drugs, including drugs in urine without a purification step, are reported using a 1 μL zero dead volume syringe in which only the analyte solution wetting the walls of the syringe needle is used in the analysis.

  6. Development and application of mass-spectrometric methods for the quantification and characterization of organic compounds in ice cores

    OpenAIRE

    Müller-Tautges, Christina

    2014-01-01

    Eisbohrkerne stellen wertvolle Klimaarchive dar, da sie atmosphärisches Aerosol konservieren. Die Analyse chemischer Verbindungen als Bestandteil atmosphärischer Aerosole in Eisbohrkernen liefert wichtige Informationen über Umweltbedingungen und Klima der Vergangenheit. Zur Untersuchung der α-Dicarbonyle Glyoxal und Methylglyoxal in Eis- und Schneeproben wurde eine neue, sensitive Methode entwickelt, die die Stir Bar Sorptive Extraction (SBSE) mit der Hochleistungsflüssigchromatographie-Masse...

  7. The detection and mapping of the spatial distribution of insect defense compounds by desorption atmospheric pressure photoionization Orbitrap mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Rejšek, Jan; Vrkoslav, Vladimír; Hanus, Robert; Vaikkinen, A.; Haapala, M.; Kauppila, T. J.; Kostiainen, R.; Cvačka, Josef

    2015-01-01

    Roč. 886, Jul 30 (2015), s. 91-97. ISSN 0003-2670 R&D Projects: GA ČR GP13-25137P Grant ostatní: GA AV ČR(CZ) M200551204 Institutional support: RVO:61388963 Keywords : desorption atmospheric pressure photoionization * ambient mass spectrometry * insect chemical defense * exocrine glands * termite * stink bug Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.513, year: 2014

  8. A review of recent advances in mass spectrometric methods for gas-phase chiral analysis of pharmaceutical and biological compounds.

    Science.gov (United States)

    Wu, Lianming; Vogt, Frederick G

    2012-10-01

    Chirality has been of great interest in pharmaceutical and biological sciences. The capabilities of mass spectrometry (MS) for rapid analysis of complex mixtures have encouraged its exploration for gas-phase chiral differentiation. Although particular instances of successful discrimination between enantiomers have been reported over the past three decades, a general method of quantitative chiral analysis by MS has only been demonstrated recently. This review describes the current state of the chiral MS methods without chiral chromatographic separation, which fall into five main categories: (1) the kinetic method, (2) host-guest (H-G) diastereomeric adduct formation, (3) ion/molecule (equilibrium) reactions, (4) collision-induced dissociation (CID) of diastereomeric adducts, and (5) the emerging technique for gas-phase separation using ion mobility spectrometry (IMS). It emphasizes tandem mass spectrometry (MS/MS), which provides several unique analytical advantages for quantitative chiral analysis. These include intrinsically high sensitivity, molecular specificity, and tolerance to impurities as well as the simplicity and speed of the mass spectrometric measurements. Practical prospects and current challenges in quantitative chiral MS techniques for QbD (quality-by-design)-based pharmaceutical applications are also discussed. PMID:22579598

  9. Effects of Conventional Heating on the Stability of Major Olive Oil Phenolic Compounds by Tandem Mass Spectrometry and Isotope Dilution Assay

    Directory of Open Access Journals (Sweden)

    Giovanni Sindona

    2010-12-01

    Full Text Available The quality of olive oils is sensorially tested by accurate and well established methods. It enables the classification of the pressed oils into the classes of extra virgin oil, virgin oil and lampant oil. Nonetheless, it would be convenient to have analytical methods for screening oils or supporting sensorial analysis using a reliable independent approach based on exploitation of mass spectrometric methodologies. A number of methods have been proposed to evaluate deficiencies of extra virgin olive oils resulting from inappropriate technological treatments, such as high or low temperature deodoration, and home cooking processes. The quality and nutraceutical value of extra virgin olive oil (EVOO can be related to the antioxidant property of its phenolic compounds. Olive oil is a source of at least 30 phenolic compounds, such as oleuropein, oleocanthal, hydroxytyrosol, and tyrosol, all acting as strong antioxidants, radical scavengers and NSAI-like drugs. We now report the efficacy of MRM tandem mass spectrometry, assisted by the isotope dilution assay, in the evaluation of the thermal stability of selected active principles of extra virgin olive oil.

  10. Measurement of mass attenuation coefficients in some Cr, Co and Fe compounds around the absorption edge and the validity of the mixture rule

    Indian Academy of Sciences (India)

    U Turgut; O Şimşek; E Büyükkasap

    2007-08-01

    The total mass attenuation coefficients for elements Cr, Co and Fe and compounds CrCl2, CrCl3, Cr2(SO4)32SO4·24H2O, CoO, CoCl2, Co(CH3COO)2, FePO4, FeCl3·6H2O, Fe(SO4)2NH4·12H2O were measured at different energies between 4.508 and 14.142 keV using secondary excitation method. Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Br, Rb, Sr were chosen as secondary exciters. 59.5 keV -rays emitted from a 241Am annular source were used to excite a secondary exciter and K (K-L3, L2) lines emitted by the secondary exciter were counted by a Si(Li) detector with a resolution of 160 eV at 5.9 keV. It was observed that mixture rule method is not a suitable method for determination of the mass attenuation coefficients of compounds, especially at an energy that is near the absorption edge. The obtained values were compared with theoretical values.

  11. Decay analysis of compound nuclei with mass A$\\sim 30-200$ formed in the reactions involving loosely bound projectiles

    CERN Document Server

    Kaur, Mandeep; Sharma, Manoj K; Gupta, Raj K

    2015-01-01

    The dynamics of the reactions forming compound nuclei using loosely bound projectiles is analysed within the framework of dynamical cluster decay model (DCM) of Gupta and Collaborators. We have analysed different reactions with $^{7}Li$, $^{9}Be$ and $^{7}Be$ as neutron rich and neutron deficient projectiles, respectively, on different targets at the three $E_{lab}$ values, forming compound nuclei within the mass region A$\\sim 30-200$. The contributions of light particles LPs ($A\\le4$) cross sections $\\sigma_{LP}$, energetically favoured intermediate mass fragments IMFs ($5 \\le A_2 \\le 20$) cross sections $\\sigma_{IMF}$ as well as fusion-fission $\\it{ff}$ cross sections $\\sigma_{ff}$ constitute the $\\sigma_{fus}$ (=$\\sigma_{LP}$+$\\sigma_{IMF}$+$\\sigma_{ff}$) for these reactions. The contribution of the emitted LPs, IMFs and ff fragments is added for all the angular momentum upto the $\\ell_{max}$ value, for the resepctive reactions. Interestingly, we find that the $\\Delta R^{emp}$, the only parameter of model ...

  12. Determination of the concentration of nitrogenous bio-organic compounds using an isotope ratio mass spectrometer operating in continuous flow mode.

    Science.gov (United States)

    Tea, Illa; Kosieradzka, Katarzyna; Antheaume, Ingrid; Gentil, Emmanuel; Robins, Richard J

    2011-09-01

    The quality of the determination of compound-specific isotopic content at natural abundance by gas chromatography-isotope ratio measurement-mass spectrometry (GC-irm-MS) relies on the stability of the voltage generated by the ion detector Faraday cages. The application of GC-irm-MS to the determination of δ(13)C (‰) and δ(15)N (‰) is now routine. However, for numerous applications, it is necessary to determine both the isotope content (δ(15)N) and the quantity (in micromoles) of analyte present. We now show that it is possible for nitrogen-containing compounds to measure how much analyte is present with an irm mass spectrometer linked to a GC by exploiting the integrated N(2) total ion current intensity (Vs) generated by measuring the (15)N/(14)N isotope ratio. The method is validated over a range of concentration (2-70 mmol/L) and δ(15)N (-70 to +50‰) values for six molecules of diverse chemical nature and functionality (nortropine, norpseudotropine, nortropinone, cysteine, taurine, glutathione). It is shown that once the ion current is calibrated, the quantitative values are of a comparable quality to those obtained from GC with flame ionization detection (GC-FID). In addition, it is demonstrated that over a definable range, the δ(15)N (‰) value is independent of the quantity of analyte introduced, confirming the validity of this method. PMID:21735067

  13. Simultaneous determination of five major compounds in the traditional medicine Pyeongwee-San by high performance liquid chromatography-diode array detection and liquid chromatography-mass spectrometry/mass spectrometry

    Directory of Open Access Journals (Sweden)

    Bohyoung Lee

    2014-01-01

    Full Text Available Background: Pyeongwee-San (PWS has been widely used for treating acute gastritis, chronic, and gastritis. Objective: In this paper, simultaneous determination of five compounds (naringin, hesperidin, glycyrrhizin, atractylenolide III, and magnolol from traditional medicine PWS using the high performance liquid chromatography (HPLC was established for quality control. Materials and Methods: Optimum separations were obtained with a SHISEIDO C18 reverse-phase column by gradient elution with 0.1% Trifluoroacetic acid (TFA water-acetonitrile as the mobile phase. The flow rate was 1 mL/min and detection wavelength was set at 205 nm and 250 nm. Validation of the analytical method was evaluated by linearity, precision, and accuracy test. Results: The calibration curves were linear over the established range with R 2 > 0.9978. The limit of detection (LOD and limit of quantification (LOQ ranged from 0.09 to 0.43 and 0.27 to 1.29 μg/mL. The method exhibited intra-day and inter-day precision range between 0.01-1.86% and 0.04-0.35% respectively. The recoveries of five compounds in PWS were in the range between 93.18-106.40%, and 0.20-1.51%. The application of this method was identified through the successful analysis of five compounds in 12 batches of PWS. In addition, identification of five compounds was confirmed by a liquid chromatography method and mass spectrometry. Conclusion: The HPLC method was could be accomplished to the quality control and stable experiment for the preparations consisted of five major compounds.

  14. Comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry for the identification of organobrominated compounds in bluefin tuna.

    Science.gov (United States)

    Pena-Abaurrea, Miren; Covaci, Adrian; Ramos, Lourdes

    2011-09-28

    This study evaluates comprehensive two-dimensional gas chromatography (GC×GC) coupled to time-of-flight mass spectrometry (GC×GC-ToF MS) for the simultaneous analysis of several classes of organobromines (OBs), including polybrominated diphenyl ethers (PBDEs), polybrominated biphenyls (PBBs), methoxylated PBDEs (MeO-PBDEs), several halogenated naturally produced compounds (HNPs) and eight novel brominated flame retardants (NBFRs), polybrominated hexahydroxanthene derivates (PBHDs), 2,4,6-tribromoanisole and a mixed halogenated compound (MHC-1), in bluefin tuna muscles. The proposed methodology maximised separation of both within and among OB families, and among these and other halogenated micropollutants detected in these samples and co-extracted matrix components. Special attention has been paid to solve co-elution problems observed during the analysis of OBs with one-dimensional GC-based techniques. Satisfactory separation among several relevant PBDEs and MeO-PBDEs has been obtained allowing their unambiguous determination in a single run. Additional studies were conducted to identify selected NBFRs and HNPs. 2,4-Dibromoanisole, a dibromophenol isomer and hexabromobenzene were identified in the investigated samples. Several new tri- and tetra-BHD derivates were also identified, indicating that these compounds could apparently exist as structured families in nature. In addition, a tetrabrominated diMeO-biphenyl and two tetrabrominated diMeO-BDEs were also tentatively identified. PMID:21872866

  15. In cleanroom, sub-ppb real-time monitoring of volatile organic compounds using proton-transfer reaction/time of flight/mass spectrometry

    Science.gov (United States)

    Hayeck, Nathalie; Maillot, Philippe; Vitrani, Thomas; Pic, Nicolas; Wortham, Henri; Gligorovski, Sasho; Temime-Roussel, Brice; Mizzi, Aurélie; Poulet, Irène

    2014-04-01

    Refractory compounds such as Trimethylsilanol (TMS) and other organic compounds such as propylene glycol methyl ether acetate (PGMEA) used in the photolithography area of microelectronic cleanrooms have irreversible dramatic impact on optical lenses used on photolithography tools. There is a need for real-time, continuous measurements of organic contaminants in representative cleanroom environment especially in lithography zone. Such information is essential to properly evaluate the impact of organic contamination on optical lenses. In this study, a Proton-Transfer Reaction-Time-of-Flight Mass spectrometer (PTR-TOF-MS) was applied for real-time and continuous monitoring of fugitive organic contamination induced by the fabrication process. Three types of measurements were carried out using the PTR-TOF-MS in order to detect the volatile organic compounds (VOCs) next to the tools in the photolithography area and at the upstream and downstream of chemical filters used to purge the air in the cleanroom environment. A validation and verification of the results obtained with PTR-TOF-MS was performed by comparing these results with those obtained with an off-line technique that is Automated Thermal Desorber - Gas Chromatography - Mass Spectrometry (ATD-GC-MS) used as a reference analytical method. The emerged results from the PTR-TOF-MS analysis exhibited the temporal variation of the VOCs levels in the cleanroom environment during the fabrication process. While comparing the results emerging from the two techniques, a good agreement was found between the results obtained with PTR-TOF-MS and those obtained with ATD-GC-MS for the PGMEA, toluene and xylene. Regarding TMS, a significant difference was observed ascribed to the technical performance of both instruments.

  16. Laboratory and Ambient Measurements of Oxidized Organic Compounds in the Gas Phase Using Nitrate Ion Chemical Ionization Coupled with High Resolution Time-of-Flight Mass Spectrometry

    Science.gov (United States)

    Massoli, P.; Stark, H.; Canagaratna, M. R.; Krechmer, J.; Lambe, A. T.; Isaacman-VanWertz, G. A.; Nowak, J. B.; Kimmel, J.; Kroll, J. H.; Jayne, J. T.; Worsnop, D. R.

    2015-12-01

    Chemical Ionization Mass Spectrometry (CIMS) is a widely used technique for molecular level characterization of inorganic and organic gas phase species. Here we present laboratory and ambient measurements of gaseous organic compounds by means of a High Resolution Time-of-Flight Chemical Ionization Mass Spectrometry (HR-ToF-CIMS) using nitrate ion (NO3-) chemistry, which recently has proven capable of selectively detecting oxidized organic molecules in the gas-phase via clustering with NO3- and its high order clusters. Such low and extremely low volatility organic compounds (LVOC, ELVOC) have an important role in particulate phase chemistry and formation of secondary organic aerosol (SOA). The HR-ToF-CIMS was deployed during the Southern Oxidant and Aerosol Study (SOAS) at the forest site in Centreville, AL (June 1 - July 15, 2013), where emissions were dominated by biogenic volatile organic compounds (BVOC), occasionally mixing with anthropogenic emissions. During SOAS, the HR-ToF-CIMS detected oxidation products of both isoprene (typically C5 LVOC) and terpenes (typically C10 ELVOC). The isoprene-related LVOC showed a diurnal cycle with a day time peak, while two groups of terpene ELVOC were identified, one peaking at night and one peaking during the day. Positive Matrix Factorization (PMF) analyses are applied to the dataset to further interpret these observations. The effect of anthropogenic pollution on the biogenic-dominated environment was also investigated during periods of elevated nitrous and sulfur dioxide levels. To further aid in interpretation of the SOAS dataset, oxidized organic molecules were produced via OH and O3 initiated oxidation of biogenic gas-phase precursors in targeted laboratory studies and detected using the HR-ToF-CIMS. Spectra were obtained in these studies over a range of simulated atmospheric conditions.

  17. A PRELIMINARY TRIAL OF THE MASS-TREATMENT OF URINARY BILHARZIASIS WITH AN ORGANO-PHOSPHORUS COMPOUND

    Directory of Open Access Journals (Sweden)

    I. Farahmandian

    1974-07-01

    Full Text Available In the course of an evaluation of various schistosomicidal drugs In Iran, the effect of an organo-phosphorus compound in the-treatment of 45 mild cases of urinary bilhariziasis was assessed and the drug was given in 3 doses of 10 mg/kg body weight each with 3-week intervals. Follow-up examinations undertaken 3 weeks after the 1st, 2nd and 3rd doses as well as 3 months after completion of therapy showed cure rates of 71, 82, 91 and 90% responsively. A reverse correlation was observed between the mean number of eggs excreted in the urine and the cure rate. Side-effects were mild and were observed in only 20% of the patients. In order of their frequency, they were abdumina1 pain, nausea, headache, vertigo and vomiting. The administration of Atropine together with each dose of the drug did not have any effect on the reduction of side-effects.

  18. Simultaneous speciation of mercury and butyltin compounds in natural waters and snow by propylation and species-specific isotope dilution mass spectrometry analysis

    Energy Technology Data Exchange (ETDEWEB)

    Monperrus, M.; Tessier, E.; Veschambre, S.; Amouroux, D.; Donard, O. [Universite de Pau et des Pays de L' Adour, Laboratoire de Chimie Analytique Bio-inorganique et Environnement, CNRS UMR 5034, Helioparc, Pau (France)

    2005-02-01

    A robust method has been developed for simultaneous determination of mercury and butyltin compounds in aqueous samples. This method is capable of providing accurate results for analyte concentrations in the picogram per liter to nanogram per liter range. The simultaneous determination of the mercury and tin compounds is achieved by species-specific isotope dilution, derivatization, and gas chromatography-inductively coupled plasma mass spectrometer (GC-ICP-MS). In derivatization by ethylation and propylation, reaction conditions such as pH and the effect of chloride were carefully studied. Ethylation was found to be more sensitive to matrix effects, especially for mercury compounds. Propylation was thus the preferred derivatization method for simultaneous determination of organomercury and organotin compounds in environmental samples. The analytical method is highly accurate and precise, with RSD values of 1 and 3% for analyte concentrations in the picogram per liter to nanogram per liter range. By use of cleaning procedures and SIDMS blank measurements, detection limits in the range 10-60 pg L{sup -1} were achieved; these are suitable for determination of background levels of these contaminants in environmental samples. This was demonstrated by using the method for analysis of real snow and seawater samples. This work illustrates the great advantage of species-specific isotope dilution for the validation of an analytical speciation method - the possibility of overcoming species transformations and non-quantitative recovery. Analysis time is saved by use of the simultaneous method, because of the use of a single sample-preparation procedure and one analysis. (orig.)

  19. Simultaneous speciation of mercury and butyltin compounds in natural waters and snow by propylation and species-specific isotope dilution mass spectrometry analysis.

    Science.gov (United States)

    Monperrus, M; Tessier, E; Veschambre, S; Amouroux, D; Donard, O

    2005-02-01

    A robust method has been developed for simultaneous determination of mercury and butyltin compounds in aqueous samples. This method is capable of providing accurate results for analyte concentrations in the picogram per liter to nanogram per liter range. The simultaneous determination of the mercury and tin compounds is achieved by species-specific isotope dilution, derivatization, and gas chromatography-inductively coupled plasma mass spectrometer (GC-ICP-MS). In derivatization by ethylation and propylation, reaction conditions such as pH and the effect of chloride were carefully studied. Ethylation was found to be more sensitive to matrix effects, especially for mercury compounds. Propylation was thus the preferred derivatization method for simultaneous determination of organomercury and organotin compounds in environmental samples. The analytical method is highly accurate and precise, with RSD values of 1 and 3% for analyte concentrations in the picogram per liter to nanogram per liter range. By use of cleaning procedures and SIDMS blank measurements, detection limits in the range 10-60 pg L(-1) were achieved; these are suitable for determination of background levels of these contaminants in environmental samples. This was demonstrated by using the method for analysis of real snow and seawater samples. This work illustrates the great advantage of species-specific isotope dilution for the validation of an analytical speciation method-the possibility of overcoming species transformations and non-quantitative recovery. Analysis time is saved by use of the simultaneous method, because of the use of a single sample-preparation procedure and one analysis. PMID:15602618

  20. Quantification of trace O-containing compounds in GTL process samples via Fischer-Tropsch reaction by comprehensive two-dimensional gas chromatography/mass spectrometry.

    Science.gov (United States)

    Fernandes, Daniella R; Pereira, Vinícius B; Stelzer, Karen T; Gomes, Alexandre O; Neto, Francisco R Aquino; Azevedo, Débora A

    2015-11-01

    Comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC-TOFMS) was successfully applied to eight real Brazilian Fischer-Tropsch (FT) product samples for the quantitative analysis of O-containing compounds. It not only allowed identifying and quantifying simultaneously a large number of O-containing compounds but also resolved many co-eluting components, such as carboxylic acids, which co-elute in one-dimensional gas chromatography. The homologous series of alcohols and carboxylic acids as trimethylsilyl derivatives were detected and identified at trace levels. The absolute quantification of each compound was accomplished with reliability using analytical curves. Linear alcohols (from C5 to C19), branched alcohols (C6-C13) and carboxylic acids (C4 to C12) were obtained in the range of 1.58 mg g(-1) to 14.75 mg g(-1), 0.51 mg g(-1) to 1.12 mg g(-1) and 0.21 mg g(-1) to 1.63 mg g(-1) of FT product samples, respectively. GC×GC-TOFMS provided a linear range (from 0.3 ng µL(-1) to 10 ng µL(-1)), good precision (<8%), and excellent accuracy (recovery range of 77% to 118%) for quantification of individual O-containing compounds in FT product samples. The results can benefit the development of gas-to-liquid technologies from natural gas and guide the choice of an FT conversion process that generates clean products with higher added value. PMID:26452870

  1. Rapid and simple determination of acrylamide in conventional cereal-based foods and potato chips through conversion to 3-[bis(trifluoroethanoyl)amino]-3-oxopropyl trifluoroacetate by gas chromatography coupled with electron capture and ion trap mass spectrometry detectors.

    Science.gov (United States)

    Russo, Mario Vincenzo; Avino, Pasquale; Centola, Angela; Notardonato, Ivan; Cinelli, Giuseppe

    2014-03-01

    A new, simple, rapid and fully validated method based on gas chromatography coupled with Electron capture and ion trap mass spectrometry detectors (GC-ECD and GC-IT/MS) is presented for quantitative analysis of acrylamide contaminant in conventional cereal-based foods and potato chips. Before analysis acrylamide was efficiently derivatized with trifluoroacetic anhydride, the effects of temperature, reaction time and catalyst on the acylation reaction were evaluated. Chromatographic analysis was performed on SE-54 capillary column; good retention and peak response of the acrylamide derivative achieved under the optimal conditions. The analytical method has been fully validated by assessment of the following parameters: LODs and LOQs (1 and 25ngg(-1) by GC-ECD and 2 and 36ngg(-1) by GC-IT/MS, with a Relative Standard Deviations potato chips). PMID:24176333

  2. Preparation of hydrotalcite compounds using ultrasound irradiation to capture CO{sub 2}; Preparacion de compuestos tipo hidrotalcita utilizando irradiacion de ultrasonido para la captura de CO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Martinez, J.A.J.; Paredes, S.P.; Valenzuela, M.A.; Hernandez, M.L. [Instituto Politecnico Nacional, ESIQIE, Mexico, D.F. (Mexico)]. E-mail: sparedesc@ipn.com.mx

    2009-09-15

    Al-Mg hydrotalcite compounds (HTC) were prepared using co-precipitation, sol-gel and reconstruction of the structure with ultrasound-assisted irradiation. The interlaminar components for each method were nitrate, acetylacetonate ethoxide and metavanadate, respectively. Optimization of the synthesis was performed using x-ray diffraction. The effect of the different parameters on synthesis was studied, including pH, time and ultrasound irradiation power. In addition, for the reconstruction method, temperature and calcination time were evaluated. For all methods, ultrasound-assisted methods were found to be more efficient and economical than conventional methods reported (autoclave). They also have the advantage of being able to control properties such as crystallinity, porosity and the specific surface, which significantly depends on the preparation method, irradiation time and type of interlaminar component. These methods are intended to synthesize interlaminar anionic materials that are very scarce in nature with better properties than traditional adsorbents used for the capture of CO{sub 2}. [Spanish] Se prepararon compuestos tipo hidrotalcita Al-Mg por los metodos de: coprecipitacion, sol gel y reconstruccion de la estructura asistidos por irradiacion de ultrasonido. Los componentes interlaminares para cada metodo fueron respectivamente: nitrato, etoxido-acetilacetonato y metavanadato. La optimizacion de la sintesis, se efectuo mediante difraccion de rayos-X. Se estudio el efecto de diversos parametros en la sintesis: pH, tiempo y potencia de irradiacion de ultrasonido, ademas, para el metodo de reconstruccion se evaluaron la temperatura y el tiempo de calcinacion. En todos los casos se encontro que el empleo de metodos asistidos por ultrasonido resultan ser mas eficientes y economicos que los metodos convencionales reportados (autoclave), ademas tienen la ventaja, de poder controlar propiedades tales como: la cristalinidad, la porosidad y la superficie

  3. Assessing levels of halogenated organic compounds in mass-stranded long-finned pilot whales (Globicephala melas) from Australia.

    Science.gov (United States)

    Weijs, Liesbeth; Tibax, Detlef; Roach, Anthony C; Manning, Therese M; Chapman, John C; Edge, Katelyn; Blust, Ronny; Covaci, Adrian

    2013-09-01

    Pollution is a threat to the health of marine mammals worldwide. Mass-strandings are poorly understood, but often involve pilot whales. However, there is limited information regarding pollution in long-finned pilot whales from Australia. Consequently, the profiles and levels of several pollutant classes were investigated in blubber of Tasmanian long-finned pilot whales. DDX levels were highest in all groups, followed by PCBs or MeO-PBDEs and lowest for PBDEs. The concentrations of all pollutants decreased with age in males. This is at least partly due to the growth dilution effect although it might also be caused by decreasing levels of PCBs, PBDEs, DDXs, HCB and CHLs in the environment. Fetus/mother ratios of higher chlorinated PCBs increased with the duration of pregnancy suggesting a preference for offloading via gestation rather than through lactation. Overall, the highest pollutant levels were found in the youngest animals. PMID:23714247

  4. Microemulsion electrokinetic chromatography with on-line atmospheric pressure photoionization-mass spectrometric detection of medium polarity compounds.

    Science.gov (United States)

    Himmelsbach, Markus; Haunschmidt, Manuela; Buchberger, Wolfgang; Klampfl, Christian W

    2007-08-01

    In this paper, we present the determination of pharmaceuticals employing microemulsion electrokinetic chromatography (MEEKC) with atmospheric pressure photoionization-mass spectrometric (APPI-MS) detection. This recent hyphenated technique allows to overcome some disadvantages of MEEKC, namely its inherent incompatibility with MS detection. Important parameters like microemulsion (ME) composition, the composition of the sheath liquid and APPI-MS detection parameters have been investigated. Using the optimized set of parameters, the eight selected substances could be detected down to concentrations between 3 mg L(-1) (phenacetin) and 41 mg L(-1) (diltiazem). Switching to the MS2 mode, the use of specific transitions for the detection of each analyte provided improved detection limits in the range of 0.6 mg L(-1) (carbamazepine) to 6 mg L(-1) (metoprolol). Calibration curves were linear over one to two orders of magnitude with correlation coefficients better than 0.98. PMID:17416381

  5. Bipolar mass spectrometry of labile coordination complexes, redox active inorganic compounds, and proteins using a glass nebulizer for sonic-spray ionization.

    Science.gov (United States)

    Antonakis, Manolis M; Tsirigotaki, Alexandra; Kanaki, Katerina; Milios, Constantinos J; Pergantis, Spiros A

    2013-08-01

    In this study, we report on the development of a novel nebulizer configuration for sonic-spray ionization (SSI) mass spectrometry (MS), more specifically for a version of SSI that is referred to as Venturi easy ambient sonic-spray ionization (V-EASI) MS. The developed nebulizer configuration is based on a commercially available pneumatic glass nebulizer that has been used extensively for aerosol formation in atomic spectrometry. In the present study, the nebulizer was modified in order to achieve efficient V-EASI-MS operation. Upon evaluating this system, it has been demonstrated that V-EASI-MS offers some distinct advantages for the analysis of coordination compounds and redox active inorganic compounds over the predominantly used electrospray ionization (ESI) technique. Such advantages, for this type of compounds, are demonstrated here for the first time. More specifically, a series of labile heptanuclear heterometallic [Cu(II) 6Ln(III)] clusters held together with artificial amino acid ligands, in addition to easily oxidized inorganic oxyanions of selenium and arsenic, were analyzed. The observed advantages pertain to V-EASI appearing to be a "milder" ionization source than ESI, not requiring electrical potentials for gas phase ion formation, thus eliminating the possibility of unwanted redox transformations, allowing for the "simultaneous" detection of negative and positive ions (bipolar analysis) without the need to change source ionization conditions, and also not requiring the use of syringes and delivery pumps. Because of such features, especially because of the absence of ionization potentials, EASI can be operated with minimal requirements for source parameter optimization. We observed that source temperature and accelerating voltage do not seem to affect labile compounds to the extent they do in ESI-MS. In addition, bipolar analysis of proteins was demonstrated here by acquiring both positive and negative ion mass spectra from the same protein solutions

  6. Carbon dioxide capture using polyethylenimine-loaded mesoporous carbons

    Institute of Scientific and Technical Information of China (English)

    Jitong Wang; Huichao Chen; Huanhuan Zhou; Xiaojun Liu; Wenming Qiao; Donghui Long; Licheng Ling

    2013-01-01

    A high efficiency sorbent for CO2 capture was developed by loading polyethylenimine (PEI) on mesoporous carbons which possessed well-developed mesoporous structures and large pore volume.The physicochemical properties of the sorbent were characterized by N2 adsorption/desorption,scanning electron microscopy (SEM),thermal gravimetric analysis (TG) and Fourier transform infrared spectroscopy (FT-IR) techniques followed by testing for CO2 capture.Factors that affected the sorption capacity of the sorbent were studied.The sorbent exhibited extraordinary capture capacity with CO2 concentration ranging from 5% to 80%.The optimal PEI loading was determined to be 65 wt.% with a CO2 sorption capacity of 4.82 mmol-CO2/g-sorbent in 15% CO2/N2 at 75℃,owing to low mass-transfer resistance and a high utilization ratio of the amine compound (63%).Moisture had a promoting effect on the sorption separation of CO2.In addition,the developed sorbent could be regenerated easily at 100℃,and it exhibited excellent regenerability and stability.These results indicate that this PEI-loaded mesoporous carbon sorbent should have a good potential for CO2 capture in the future.

  7. Determination of polybrominated diphenyl ethers in house dust using standard addition method and gas chromatography with electron capture and mass spectrometric detection.

    Science.gov (United States)

    Król, Sylwia; Zabiegała, Bożena; Namieśnik, Jacek

    2012-08-01

    Monitoring of the environmental fate of polybrominated diphenyl ethers (PBDEs) involves determination of their concentration in air, airborne particles and settled dust. This requires the implementation of appropriate analytical tools like measuring instruments, reference materials and analytical procedures. In this study an analytical procedure was developed for determining PBDEs in samples with a complex matrix composition. The efficiencies of three different extraction techniques - Soxhlet extraction (SE), Accelerated Solvent Extraction (ASE) and Ultrasound Assisted Extraction (UAE) - were compared. The study investigated the possibility of using the standard addition method for estimating PBDEs levels. The GC-μECD system was successfully applied as an alternative to low resolution mass spectrometry (LRMS) for determining BDE-209 in dust samples. The developed analytical procedure was then used to analyze dust samples, collected from houses and computer suites in the Tri-city area (Gdansk, Gdynia and Sopot), in order to detect and quantify the presence of polybrominated diphenyl ethers (PBDEs) in the indoor environment. Concentrations of studied congeners (from triBDE to heptaBDE), obtained by chromatographic analysis of dust samples extracts, performed applying two measurement systems (GC-EIMS and GC-μECD) ranged between 331 and 3102 ng g(-1) for house dust and between

  8. A novel approach for identification of biologically active phenolic compounds in complex matrices using hybrid quadrupole-orbitrap mass spectrometer: A promising tool for testing antimicrobial activity of hops.

    Science.gov (United States)

    Dušek, Martin; Jandovská, Vladimíra; Čermák, Pavel; Mikyška, Alexandr; Olšovská, Jana

    2016-08-15

    The phenolic compounds, secondary metabolites of hops represent a large family of compounds that could be subsequently divided into smaller groups based on the similarities between their chemical structures. The antibacterial, antifungal and antiviral properties of hops are well known, but there is a lack of information about antimicrobial activities of individual hop compounds. This study was carried out with an objective to identify compounds present in hops that have potential antibacterial activity. In the first stage of experiment, the active compounds with potential anti-microbial activity had to be extracted from hop cones. Therefore, minced hop cones were applied on solid growth medium inoculated with Staphylococcus aureus. The active substances that migrated into the medium created an inhibition zone. In the second stage of experiment, the inhibition zones were cut out from Petri dishes, active compounds were extracted from these zones and consequently analyzed using LC-HRMS. These complex assays were developed and optimized. The data were acquired by using a quadrupole-orbitrap hybrid mass spectrometer by targeted-MS2 experiment in both ionization modes. The MS method has been developed as a screening method with a subsequent fragmentation of compound of interest on the base of inclusion mass list. The unknown compounds extracted from inhibition zones have been identified either by searching against a database or their structure has been elucidated on the basis of their fragmentation spectra. On the basis of this experiment the list of active compounds with potential anti-microbial activities was enhanced. PMID:27260455

  9. Simultaneous analysis of non-steroidal anti-inflammatory drugs and estrogenic hormones in water and wastewater samples using gas chromatography-mass spectrometry and gas chromatography with electron capture detection

    Energy Technology Data Exchange (ETDEWEB)

    Migowska, Natalia; Caban, Magda; Stepnowski, Piotr; Kumirska, Jolanta, E-mail: kumirska@chem.univ.gda.pl

    2012-12-15

    Non-steroidal anti-inflammatory drugs are the group of pharmaceuticals that is most often found in the environment, whereas estrogenic hormones are considered to be potent endocrine disruptors. However, the fate and persistence of these compounds in the environment are still unclear. In this study we propose two approaches for determining these compounds in environmental water samples: GC-MS using time windows and operating in selected ion-monitoring mode (SIM) and, for the first time, gas chromatography with electron capture detection (GC-ECD). The identification criteria of both methods fulfilled the requirements of Directive 2002/657/EC. The use of time windows improved the sensitivity of GC-MS measurements. In GC-MS analysis the pharmaceuticals were determined as trimethylsilyl, in GC-ECD as pentafluoropropionyl derivatives. The influence of such parameters as the type of reagent, type of solvent, reaction time, reaction temperature and microwave irradiation in a household microwave oven on the efficacy of silylation was investigated. Derivatization using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and 1% trimethylchlorosilane (TMCS) in pyridine (1:1, v/v) for 30 min in 60 Degree-Sign C was found to be optimal. Optimization of the solid phase extraction procedure (SPE) confirmed that the application of Oasis HLB cartridges, the acidification of loading samples to pH 2 and the use of methanol as eluent gave the best absolute recoveries (ARs) of the target compounds. The following ARs of all the compounds were achieved: 58.2-106.8% in influent wastewater, 77.8-103.4% in effluent wastewater and 81.2-101.9% in surface water samples. Validation of the SPE-GC-MS method enables 13 pharmaceuticals to be determined with MDLs between 3.3 and 343.6 ng/L, depending on the analytes and matrices. GC-ECD analysis enables the determination of 6 pharmaceuticals in surface water samples with MDLs between 0.7 and 5.4 ng/L. The proposed methods were successfully used for

  10. Simultaneous analysis of non-steroidal anti-inflammatory drugs and estrogenic hormones in water and wastewater samples using gas chromatography–mass spectrometry and gas chromatography with electron capture detection

    International Nuclear Information System (INIS)

    Non-steroidal anti-inflammatory drugs are the group of pharmaceuticals that is most often found in the environment, whereas estrogenic hormones are considered to be potent endocrine disruptors. However, the fate and persistence of these compounds in the environment are still unclear. In this study we propose two approaches for determining these compounds in environmental water samples: GC–MS using time windows and operating in selected ion-monitoring mode (SIM) and, for the first time, gas chromatography with electron capture detection (GC–ECD). The identification criteria of both methods fulfilled the requirements of Directive 2002/657/EC. The use of time windows improved the sensitivity of GC–MS measurements. In GC–MS analysis the pharmaceuticals were determined as trimethylsilyl, in GC–ECD as pentafluoropropionyl derivatives. The influence of such parameters as the type of reagent, type of solvent, reaction time, reaction temperature and microwave irradiation in a household microwave oven on the efficacy of silylation was investigated. Derivatization using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and 1% trimethylchlorosilane (TMCS) in pyridine (1:1, v/v) for 30 min in 60 °C was found to be optimal. Optimization of the solid phase extraction procedure (SPE) confirmed that the application of Oasis HLB cartridges, the acidification of loading samples to pH 2 and the use of methanol as eluent gave the best absolute recoveries (ARs) of the target compounds. The following ARs of all the compounds were achieved: 58.2–106.8% in influent wastewater, 77.8–103.4% in effluent wastewater and 81.2–101.9% in surface water samples. Validation of the SPE–GC–MS method enables 13 pharmaceuticals to be determined with MDLs between 3.3 and 343.6 ng/L, depending on the analytes and matrices. GC–ECD analysis enables the determination of 6 pharmaceuticals in surface water samples with MDLs between 0.7 and 5.4 ng/L. The proposed methods were successfully

  11. Performance evaluation using a three compartment mass balance for the removal of volatile organic compounds in pilot scale constructed wetlands.

    Science.gov (United States)

    Seeger, Eva M; Reiche, Nils; Kuschk, Peter; Borsdorf, Helko; Kaestner, Matthias

    2011-10-01

    To perform a general assessment of treatment efficiency, a mass balance study was undertaken for two types of constructed wetlands (CWs), planted gravel filters and plant root mat systems, for treating VOC (benzene; MTBE) polluted groundwater under field conditions. Contaminant fate was investigated in the respective water, plant, and atmosphere compartments by determining water and atmospheric contaminant loads and calculating contaminant plant uptake, thereby allowing for an extended efficiency assessment of CWs. Highest total VOC removal was achieved during summer, being pronounced for benzene compared to MTBE. According to the experimental results and the calculations generated by the balancing model, degradation in the rhizosphere and plant uptake accounted for the main benzene removal processes, of 76% and 13% for the gravel bed CW and 83% and 11% for the root mat system. Volatilization flux of benzene and MTBE was low (balances that allow for conclusive quantitative estimation of contaminant elimination and distribution processes (e.g., total, surface, and phytovolatilization, plant uptake, rhizodegradation) in CWs under field conditions. PMID:21848285

  12. Ultra-Sensitive Elemental Analysis Using Plasmas 5.Speciation of Arsenic Compounds in Biological Samples by High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry System

    Science.gov (United States)

    Kaise, Toshikazu

    Arsenic originating from the lithosphere is widely distributed in the environment. Many arsenicals in the environment are in organic and methylated species. These arsenic compounds in drinking water or food products of marine origin are absorbed in human digestive tracts, metabolized in the human body, and excreted viatheurine. Because arsenic shows varying biological a spects depending on its chemical species, the biological characteristics of arsenic must be determined. It is thought that some metabolic pathways for arsenic and some arsenic circulation exist in aqueous ecosystems. In this paper, the current status of the speciation analysis of arsenic by HPLC/ICP-MS (High Performance Liquid Chromatography-Inductively Coupled Plasma Mass spectrometry) in environmental and biological samples is summarized using recent data.

  13. Fermi-surface topology and field-dependent effective masses of the filled skutterudite compound PrOs{sub 4}As{sub 12}

    Energy Technology Data Exchange (ETDEWEB)

    Singleton, J. [National High Magnetic Field Laboratory, Los Alamos National Laboratory, MS-E536, Los Alamos, New Mexico 87545 (United States)], E-mail: jsingle@lanl.gov; Ho, Pei-Chun; Maple, M.B. [Department of Physics and Institute for Pure and Applied Physical Sciences, University of California, San Diego, 9500 Gilman Drive, Dept. 0360, La Jolla, CA 92093-0360 (United States); Harima, Hisatomo [Kobe University, 1-1 Rokko-dai Noda, Kobe 657-8501 (Japan); Goddard, P.A. [Clarendon Laboratory, Oxford University, Parks Road, Oxford OX1 3PU (United Kingdom); Henkie, Z. [Institute for Low Temperature and Structure Research, Polish Academy of Sciences, 50-950, Wroclaw (Poland)

    2008-04-01

    We report magnetic-field-orientation dependent de Haas-van Alphen (dHvA) experiments on the filled skutterudites PrOs{sub 4}As{sub 12} and LaOs{sub 4}As{sub 12}. The Fermi surfaces of the compounds are very similar and in reasonable agreement with bandstructure calculations for LaOs{sub 4}As{sub 12} on a PrOs{sub 4}As{sub 12} lattice. This suggests that the 4f electrons are essentially localized in the paramagnetic phase of PrOs{sub 4}As{sub 12}. Whilst the properties of LaOs{sub 4}As{sub 12} suggest a conventional nonmagnetic Fermi liquid, the effects of direct exchange and electron correlations cause dHvA beat frequencies and field-dependent quasiparticle masses in PrOs{sub 4}As{sub 12}.

  14. Fermi-surface topology and field-dependent effective masses of the filled skutterudite compound PrOs4As12

    International Nuclear Information System (INIS)

    We report magnetic-field-orientation dependent de Haas-van Alphen (dHvA) experiments on the filled skutterudites PrOs4As12 and LaOs4As12. The Fermi surfaces of the compounds are very similar and in reasonable agreement with bandstructure calculations for LaOs4As12 on a PrOs4As12 lattice. This suggests that the 4f electrons are essentially localized in the paramagnetic phase of PrOs4As12. Whilst the properties of LaOs4As12 suggest a conventional nonmagnetic Fermi liquid, the effects of direct exchange and electron correlations cause dHvA beat frequencies and field-dependent quasiparticle masses in PrOs4As12

  15. Determination of selected polycyclic aromatic compounds in particulate matter: a validation study of an agitation extraction method for samples with low mass loadings using reduced volumes

    Science.gov (United States)

    García-Alonso, S.; Pérez-Pastor, R. M.; Archilla-Prat, V.; Rodríguez-Maroto, J.; Izquierdo-Díaz, M.; Rojas, E.; Sanz, D.

    2015-12-01

    A simple analytical method using low volumes of solvent for determining selected PAHs and NPAHs in PM samples is presented. The proposed extraction method was compared with pressurized fluid (PFE) and microwave (MC) extraction techniques and intermediate precision associated to analytical measurements were estimated. Extraction by agitation with 8 mL of dichloromethane yielded recoveries above 80% compared to those obtained from PFE extraction. Regarding intermediate precision results, values between 10-20% were reached showing increases of dispersion for compounds with high volatility and low levels of concentration. Within the framework of the INTA/CIEMAT research agreement for the PM characterization in gas turbine exhaust, the method was applied for analysis of aluminum foil substrates and quartz filters with mass loading ranged from 0.02 to 2 mg per sample.

  16. Theory and Application of Dissociative Electron Capture in Molecular Identification

    CERN Document Server

    Havey, C D; Jones, T; Voorhees, K J; Laramee, J A; Cody, R B; Clougherty, D P; Eberhart, Mark; Voorhees, Kent J.; Laramee, James A.; Cody, Robert B.; Clougherty, Dennis P.

    2006-01-01

    The coupling of an electron monochromator (EM) to a mass spectrometer (MS) has created a new analytical technique, EM-MS, for the investigation of electrophilic compounds. This method provides a powerful tool for molecular identification of compounds contained in complex matrices, such as environmental samples. EM-MS expands the application and selectivity of traditional MS through the inclusion of a new dimension in the space of molecular characteristics--the electron resonance energy spectrum. However, before this tool can realize its full potential, it will be necessary to create a library of resonance energy scans from standards of the molecules for which EM-MS offers a practical means of detection. Here, an approach supplementing direct measurement with chemical inference and quantum scattering theory is presented to demonstrate the feasibility of directly calculating resonance energy spectra. This approach makes use of the symmetry of the transition-matrix element of the captured electron to discriminat...

  17. Experimental validation of an effective carbon number-based approach for the gas chromatography-mass spectrometry quantification of 'compounds lacking authentic standards or surrogates'.

    Science.gov (United States)

    Kim, Yong-Hyun; Kim, Ki-Hyun; Szulejko, Jan E; Bae, Min-Suk; Brown, Richard J C

    2014-06-01

    For the quantitative analysis of 'compounds lacking authentic standards or surrogates' (CLASS) in environmental media, we previously introduced an effective carbon number (ECN) approach to develop an empirical equation for the prediction of their response factor (RF). In this research, a series of laboratory experiments were carried out to benchmark the reliability of an ECN approach for sorbent tube/thermal desorption/gas chromatography (GC)/mass spectrometry (MS) applications. First, the ECN values were determined using external calibration data from 25 reference volatile organic compounds (VOCs) using two MS dectectors (quadrupole (Q) and time-of-flight (TOF)). Then, a certified standard mixture of 54 VOCs was analyzed by each system as a simulated unknown sample. The analytical bias, assessed in terms of percentage difference (PD) between the certified and ECN-predicted mass values, averaged 19.2±16.1% (TOF-MS) and 28.2±27.6% (Q-MS). The bias using a more simplified carbon number (CN)-based prediction increased considerably, yielding 53.4±53.3% (TOF-MS) and 61.7±81.3% (Q-MS). However, the bias obtained using the ECN-based prediction decreased significantly to yield average PD values of 9.84±7.28% (TOF-MS) and 16.8±8.35% (Q-MS), if the comparison was limited to 26 (out of 54) VOCs with CN≥4 (i.e., 25 aromatics and hexachlorobutadiene). PMID:24856509

  18. Measurements of Oxidized Organic Compounds during SOAS 2013 using nitrate ion chemical ionization coupled with High Resolution Time-of-Flight Mass Spectrometry

    Science.gov (United States)

    Massoli, P.; Stark, H.; Cnagaratna, M.; Junninen, H.; Hakala, J. P.; Mauldin, R.; Ehn, M.; Sipila, M.; Krechmer, J.; Kimmel, J.; Jimenez, J. L.; Jayne, J. T.; Worsnop, D. R.

    2013-12-01

    We present ambient measurements of gaseous organic compounds by means of a High Resolution Time-of-Flight Chemical Ionization Mass Spectrometry (HR-ToF-CIMS) using nitrate ion (NO3-) chemistry. This technique allows to selectively detect oxidized gas-phase species, e.g., oxidized organic molecules and sulfuric acid via clustering with NO3- and its high order clusters. The capability of making such measurements is important because both sulfuric acid and organic gas molecules have a recognized key role in new particle formation (NPF) processes and likely have an important role in particulate phase chemistry and formation of secondary organic aerosols (SOA). The HR-ToF-CIMS was deployed during the Southern Oxidant and Aerosol Study (SOAS) at the forest supersite in Centreville, AL, from June 1 to July 15, 2013. The main goal of the SOAS campaign was to investigate the composition and sources of SOA in the Southeast US, where emissions are mainly represented by biogenic volatile organic compounds (BVOC) emissions and in less extent by anthropogenic emissions (AVOC). During SOAS, the HR-ToF-CIMS detected a range of organic ions that based on previous literature could be identified as oxidation products of both isoprene and terpenes. The isoprene products were 5 to 10 times more abundant than the terpene products. The isoprene-related molecules showed a diurnal cycle with a day time peak, typically after 1500 local time, while the terpene products were higher at night (between 2000 and 0600 local time). These results are consistent with the diurnal trends of primary BVOC emissions from other co-located instruments. The ambient data are also compared to laboratory measurements where oxidized organic vapors are produced using a Potential Aerosol Mass (PAM) flow reactor by the OH oxidation of biogenic gas-phase precursors (isoprene, a-pinene) over multiple days of equivalent atmospheric exposure.

  19. Analysis of endocrine disrupters and related compounds in sediments and sewage sludge using on-line turbulent flow chromatography-liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Gorga, Marina; Insa, Sara; Petrovic, Mira; Barceló, Damià

    2014-07-25

    A novel fully automated method based on dual column switching using turbulent flow chromatography followed by liquid chromatography coupled to tandem mass spectrometry (TFC-LC-MS/MS) was applied for the determination of endocrine disruptors (EDCs) and related compounds in sediment and sewage sludge samples. This method allows the unequivocal identification and quantification of the most relevant environmental EDCs such as natural and synthetic estrogens and their conjugates, antimicrobials, parabens, bisphenol A (BPA), alkylphenolic compounds, benzotriazoles, and organophosphorus flame retardants, minimizing time of analysis and alleviating matrix effects. Applying this technique, after the extraction of the target compounds by pressurized liquid extraction (PLE), sediment and sewage sludge extracts were directly injected to the chromatographic system and the analytes were concentrated into the clean-up loading column. Using six-port switching system, the analytes were transferred to the analytical column for subsequent detection by MS-MS (QqQ). In order to optimize this multiplexing system, a comparative study employing six types of TurboFlow™ columns, with different chemical modifications, was performed to achieve the maximum retention of analytes and best elimination of matrix components. Using the optimized protocol low limits of quantification (LOQs) were obtained ranging from 0.0083 to 1.6 ng/g for sediment samples and from 0.10 to 125 ng/g for sewage sludge samples (except for alkylphenol monoethoxylate). The method was used to evaluate the presence and fate of target EDCs in the Ebro River which is the most important river in Spain with intensive agricultural and industrial activities in the basin that contribute to deteriorating soil and water quality. PMID:24909438

  20. Preparation and mass spectrometrical high temperature investigations on compounds of the quasi-ternary system Cs2O-Al2O3-SiO2

    International Nuclear Information System (INIS)

    Additions of aluminium oxide and silicen oxide to ceramic fuel for pyrocarbon-coated nuclear fuel paticles counteract a release of fission-cesium by compound formation. The vapourization tests carried out here using samples from the quasi-ternary system cesium-oxide-aluminium-oxide-silicon-oxide by means of high-temperature mass spectroscopy using a Knudsen cell served the optimization of this retention effect. The aim of the apparative changes on the knudsen cell were to shield heat radiation on the temperature measuring borehole through the tungsten wire cathode in order to be able to perform exact temperature measurements even below 1,0000C. A new method of preparation was developed to obtain defined cesium aluminium silicates whose composition was determined by Guinier and goniometer pictures as well as by microscopic investigations. According to the latter, 3 ternary compounds are present in the system investigated: CsAlSiO4, CsAlSi2O6 and CsAlSi5O12. Their lattice constants were determined from goniometric measurements; the vapour pressure equection were set up from the measured cesium vapour pressure values over each sample and the enthalpies of the vapourization reactions were found to be 84 kcal for CsAlSiO4 at 1,4000K, 100 kcal for CsAlSi2O6 at 1,5500K and 122 kcal for CsAlSi5O12 at 1,6500K. The cesium vapour pressures of the glas phases investigated of the system are above the Cs partial pressures of the solid crystalline phases of the same composition. The results of the work explain the causes of the reduction of the Cs release and show that the vapour pressure can be lowered by more than 10 orders of magnitude at reactor relevant temperatures by compound formation. (RB)

  1. Screening for anabolic steroids and related compounds in illegal cocktails by liquid chromatography/time-of-flight mass spectrometry and liquid chromatography/quadrupole time-of-flight tandem mass spectrometry with accurate mass measurement

    NARCIS (Netherlands)

    Nielen, M.W.F.; Vissers, J.P.C.; Fuchs, R.E.M.; Velde, van J.W.; Lommen, A.

    2001-01-01

    Findings of illegal hormone preparations such as syringes, bottles, cocktails, and so on, are an important information source for the nature of the current abuse of anabolic steroids and related compounds as growth-promoting agents in cattle. A new screening method for steroids in cocktails is prese

  2. Optimization of a Differential Ion Mobility Spectrometry-Tandem Mass Spectrometry Method for High-Throughput Analysis of Nicotine and Related Compounds: Application to Electronic Cigarette Refill Liquids.

    Science.gov (United States)

    Regueiro, Jorge; Giri, Anupam; Wenzl, Thomas

    2016-06-21

    Fast market penetration of electronic cigarettes is leading to an exponentially growing number of electronic refill liquids with different nicotine contents and an endless list of flavors. Therefore, rapid and simple methods allowing a fast screening of these products are necessary to detect harmful substances which can negatively impact the health of consumers. In this regard, the present work explores the capabilities of differential ion mobility spectrometry coupled to tandem mass spectrometry for high-throughput analysis of nicotine and 11 related compounds in commercial refill liquids for electronic cigarettes. The influence of main factors affecting the ion mobility separation, such as modifier types and concentration, separation voltage, and temperature, was systematically investigated. Despite small molecular weight differences among the studied compounds, a good separation was achieved in the ion mobility cell under the optimized conditions, which involved the use of ethanol as a polar gas-phase chemical modifier. Indeed, differential ion mobility was able to resolve (resolution >4) nicotine from its structural isomer anabasine without the use of any chromatographic separation. The quantitative performance of the proposed method was then evaluated, showing satisfactory precision (RSD ≤ 16%) and recoveries ranging from 85 to 100% for nicotine, and from 84 to 126% for the rest of the target analytes. Several commercial electronic cigarette refill liquids were analyzed to demonstrate the applicability of the method. In some cases, significant differences were found between labeled and measured levels of nicotine. Anatabine, cotinine, myosmine, and nornicotine were also found in some of the analyzed samples. PMID:27173877

  3. Mass Balance of Fipronil and Total Toxicity of Fipronil-Related Compounds in Process Streams during Conventional Wastewater and Wetland Treatment

    Science.gov (United States)

    2015-01-01

    Attenuation of the pesticide fipronil and its major degradates was determined during conventional wastewater treatment and wetland treatment. Analysis of flow-weighted composite samples by liquid and gas chromatography–tandem mass spectrometry showed fipronil occurrence at 12–31 ng/L in raw sewage, primary effluent, secondary effluent, chlorinated effluent, and wetland effluent. Mean daily loads of total fipronil related compounds in raw sewage and in plant effluent after chlorination were statistically indistinguishable (p = 0.29; n = 10), whereas fipronil itself was partially removed (25 ± 3%; p = 0.00025; n = 10); the associated loss in toxicity was balanced by the formation of toxic fipronil degradates, showing conventional treatment to be unfit for reducing overall toxicity. In contrast to these findings at the municipal wastewater treatment, both parental fipronil and the sum of fipronil-related compounds were removed in the wetland with efficiencies of 44 ± 4% and 47 ± 13%, respectively. Total fipronil concentrations in plant effluent (28 ± 6 ng/L as fipronil) were within an order of magnitude of half-maximal effective concentrations (EC50) of nontarget invertebrates. This is the first systematic assessment of the fate of fipronil and its major degradates during full-scale conventional wastewater and constructed wetland treatment. PMID:26710933

  4. Mass Balance of Fipronil and Total Toxicity of Fipronil-Related Compounds in Process Streams during Conventional Wastewater and Wetland Treatment.

    Science.gov (United States)

    Supowit, Samuel D; Sadaria, Akash M; Reyes, Edward J; Halden, Rolf U

    2016-02-01

    Attenuation of the pesticide fipronil and its major degradates was determined during conventional wastewater treatment and wetland treatment. Analysis of flow-weighted composite samples by liquid and gas chromatography-tandem mass spectrometry showed fipronil occurrence at 12-31 ng/L in raw sewage, primary effluent, secondary effluent, chlorinated effluent, and wetland effluent. Mean daily loads of total fipronil related compounds in raw sewage and in plant effluent after chlorination were statistically indistinguishable (p = 0.29; n = 10), whereas fipronil itself was partially removed (25 ± 3%; p = 0.00025; n = 10); the associated loss in toxicity was balanced by the formation of toxic fipronil degradates, showing conventional treatment to be unfit for reducing overall toxicity. In contrast to these findings at the municipal wastewater treatment, both parental fipronil and the sum of fipronil-related compounds were removed in the wetland with efficiencies of 44 ± 4% and 47 ± 13%, respectively. Total fipronil concentrations in plant effluent (28 ± 6 ng/L as fipronil) were within an order of magnitude of half-maximal effective concentrations (EC50) of nontarget invertebrates. This is the first systematic assessment of the fate of fipronil and its major degradates during full-scale conventional wastewater and constructed wetland treatment. PMID:26710933

  5. Cleaning verification assays for highly potent compounds by high performance liquid chromatography mass spectrometry: strategy, validation, and long-term performance.

    Science.gov (United States)

    Liu, Li; Pack, Brian W

    2007-03-12

    A cleaning-verification assay was validated for a highly potent family of compounds utilizing a swab-sampling procedure and high performance liquid chromatography mass spectrometry (LC-MS) for separation and detection of the analytes. Due to the high potency of the compound, the LC-MS method was validated at a level of 50 ng/25 cm(2) and 50 ng/100 cm(2) (which equates to 10 ng/ml after extraction in 5 ml of sample solvent, and 3 ng/ml after correction for sampling losses). This validation exercise included recovery estimates from all drug product contact surfaces within the clinical trial manufacturing equipment, namely, stainless steel, anodized aluminum, Rilsan coated aluminum, bronze, polyvinylchloride, and Oilon. The limit of detection for the LC-MS method was determined to be less than 0.5 ng/ml, or less than 0.1 ng/cm(2), of the analyte. This method does not employ an internal standard. Long-term performance of the validated method is also reported. The precision on replicate injections of the standard prepared in the range of 3-6 ng/ml was typically better than 8.0% relative standard deviation (R.S.D.) over the course of 1 year, which resulted from 10 cleaning-verification submissions. Those results were consistent with the data obtained during method validation. PMID:17156961

  6. Rapid gas chromatographic analysis of less abundant compounds in distilled spirits by direct injection with ethanol-water venting and mass spectrometric data deconvolution.

    Science.gov (United States)

    Macnamara, Kevin; Lee, Michelle; Robbat, Albert

    2010-01-01

    The principal trace secondary compounds common to fermentation-derived distilled spirits can be rapidly quantified by directly injecting 5muL of spirit without sample preparation to a narrow-bore 0.15mm internal diameter capillary column. The ethanol-water is removed in an initial solvent venting step using a programmed temperature vapourization injector, followed by splitless transfer of the target analytes to the column. The larger injection facilitates trace analysis and ethanol-water removal extends column lifetime. Problems of coelution between analytes or with sample matrix were surmounted by using mass spectral deconvolution software for quantification. All operations in the analysis from injection with solvent venting to data reduction are fully automated for unattended sequential sample analysis. The synergy of the various contributory steps combines to offer an effective novel solution for this analysis. Applications include quantification of low ppm amounts of acids and esters and sub-ppm profiling of trace compounds from both the raw material malt and the ageing in wood barrels. PMID:19959175

  7. Determination of Earthy-musty Odorous Compounds in Drinking Water by Vortex Assisted Dispersive Liquid-Liquid Microextraction Combined with Gas Chromatography Tandem Mass Spectrometry.

    Science.gov (United States)

    Lu, Jian; Wu, Zhong-Ping; Che, Wen-Jun; Xian, Yan-Ping; Guo, Xin-Dong; Lv, Jia-Xin; Li, He

    2016-01-01

    A new method was developed for the determination of eight earthy-musty compounds in drinking water by gas chromatography tandem mass spectrometry (GC-MS/MS) combined with dispersive liquid-liquid microextraction (DLLME). In this work, the type and volume of extraction solvent and dispersion agent, and the amount of NaCl were optimized; the linearity, detection limit, recovery and precision of method were investigated. The results indicated that the target analytes were in the range of 0.2 - 100 μg/L with correlation coefficient (r) ranging from 0.9991 to 0.9999, the limit of detection (LOD, S/N = 3) of the analytes ranged from 0.2 to 1.0 ng/L with the enrichment factor of 320. The mean recoveries for drinking water at three spiked concentrations levels of 0.6 - 32 ng/L were in the range of 91.3 to 103%, the precision ranged from 3.1 to 7.5% (n = 6), and the inter-day precision was from 6.1 to 11.1% (n = 5). Only one of 15 selected real samples tested positive for GSM, and the concentration was 3 ng/L. This method was confirmed to be simple, fast, efficient, and accurate for the determination of earthy-musty compounds in aqueous samples. PMID:27063712

  8. Improvement of a headspace solid phase microextraction-gas chromatography/mass spectrometry method for the analysis of wheat bread volatile compounds.

    Science.gov (United States)

    Raffo, Antonio; Carcea, Marina; Castagna, Claudia; Magrì, Andrea

    2015-08-01

    An improved method based on headspace solid phase microextraction combined with gas chromatography-mass spectrometry (HS-SPME/GC-MS) was proposed for the semi-quantitative determination of wheat bread volatile compounds isolated from both whole slice and crust samples. A DVB/CAR/PDMS fibre was used to extract volatiles from the headspace of a bread powdered sample dispersed in a sodium chloride (20%) aqueous solution and kept for 60min at 50°C under controlled stirring. Thirty-nine out of all the extracted volatiles were fully identified, whereas for 95 other volatiles a tentative identification was proposed, to give a complete as possible profile of wheat bread volatile compounds. The use of an array of ten structurally and physicochemically similar internal standards allowed to markedly improve method precision with respect to previous HS-SPME/GC-MS methods for bread volatiles. Good linearity of the method was verified for a selection of volatiles from several chemical groups by calibration with matrix-matched extraction solutions. This simple, rapid, precise and sensitive method could represent a valuable tool to obtain semi-quantitative information when investigating the influence of technological factors on volatiles formation in wheat bread and other bakery products. PMID:26118802

  9. Computational and Experimental Assessment of Benzene Cation Chemistry for the Measurement of Marine Derived Biogenic Volatile Organic Compounds with Chemical Ionization Mass Spectrometry

    Science.gov (United States)

    Zoerb, M.; Kim, M.; Zimmermann, K.; Bertram, T. H.

    2013-12-01

    Chemical ionization mass spectrometry (CIMS) is a highly selective and sensitive technique for the measurement of trace gases in the atmosphere. However, competing side reactions and dependence on relative humidity (RH) can make the transition from the laboratory to the field challenging. Effective implementation of chemical ionization requires a thorough knowledge of the elementary steps leading to ionization of the analyte. We have recently investigated benzene cations for the detection of marine derived biogenic volatile organic compounds (BVOCs), such isoprene and terpene compounds, from algal bloom events. Our experimental results indicate that benzene ion chemistry is an attractive candidate for field measurements, and the RH dependence is weak. To further understand the advantages and limitations of this approach, we have also used electronic structure theory calculations to compliment the experimental work. These theoretical methods can provide valuable insight into the physical chemistry of ion molecule reactions including thermodynamical information, the stability of ions to fragmentation, and potential sources of interference such as dehydration to form isobaric ions. The combined experimental and computational approach also allows validation of the theoretical methods and will provide useful information towards gaining predictive power for the selection of appropriate reagent ions for future experiments.

  10. Biodistribution and Subcellular Localization of an Unnatural Boron-Containing Amino Acid (Cis-ABCPC) by Imaging Secondary Ion Mass Spectrometry for Neutron Capture Therapy of Melanomas and Gliomas

    Science.gov (United States)

    Chandra, Subhash; Barth, Rolf F.; Haider, Syed A.; Yang, Weilian; Huo, Tianyao; Shaikh, Aarif L.; Kabalka, George W.

    2013-01-01

    The development of new boron-delivery agents is a high priority for improving the effectiveness of boron neutron capture therapy. In the present study, 1-amino-3-borono-cyclopentanecarboxylic acid (cis-ABCPC) as a mixture of its L- and D- enantiomers was evaluated in vivo using the B16 melanoma model for the human tumor and the F98 rat glioma as a model for human gliomas. A secondary ion mass spectrometry (SIMS) based imaging instrument, CAMECA IMS 3F SIMS Ion Microscope, was used for quantitative imaging of boron at 500 nm spatial resolution. Both in vivo and in vitro studies in melanoma models demonstrated that boron was localized in the cytoplasm and nuclei with some cell-to-cell variability. Uptake of cis-ABCPC in B16 cells was time dependent with a 7.5:1 partitioning ratio of boron between cell nuclei and the nutrient medium after 4 hrs. incubation. Furthermore, cis-ABCPC delivered boron to cells in all phases of the cell cycle, including S-phase. In vivo SIMS studies using the F98 rat glioma model revealed an 8:1 boron partitioning ratio between the main tumor mass and normal brain tissue with a 5:1 ratio between infiltrating tumor cells and contiguous normal brain. Since cis-ABCPC is water soluble and can cross the blood-brain-barrier via the L-type amino acid transporters (LAT), it may accumulate preferentially in infiltrating tumor cells in normal brain due to up-regulation of LAT in high grade gliomas. Once trapped inside the tumor cell, cis-ABCPC cannot be metabolized and remains either in a free pool or bound to cell matrix components. The significant improvement in boron uptake by both the main tumor mass and infiltrating tumor cells compared to those reported in animal and clinical studies of p-boronophenylalanine strongly suggest that cis-ABCPC has the potential to become a novel new boron delivery agent for neutron capture therapy of gliomas and melanomas. PMID:24058680

  11. Biodistribution and subcellular localization of an unnatural boron-containing amino acid (cis-ABCPC by imaging secondary ion mass spectrometry for neutron capture therapy of melanomas and gliomas.

    Directory of Open Access Journals (Sweden)

    Subhash Chandra

    Full Text Available The development of new boron-delivery agents is a high priority for improving the effectiveness of boron neutron capture therapy. In the present study, 1-amino-3-borono-cyclopentanecarboxylic acid (cis-ABCPC as a mixture of its L- and D-enantiomers was evaluated in vivo using the B16 melanoma model for the human tumor and the F98 rat glioma as a model for human gliomas. A secondary ion mass spectrometry (SIMS based imaging instrument, CAMECA IMS 3F SIMS Ion Microscope, was used for quantitative imaging of boron at 500 nm spatial resolution. Both in vivo and in vitro studies in melanoma models demonstrated that boron was localized in the cytoplasm and nuclei with some cell-to-cell variability. Uptake of cis-ABCPC in B16 cells was time dependent with a 7.5:1 partitioning ratio of boron between cell nuclei and the nutrient medium after 4 hrs. incubation. Furthermore, cis-ABCPC delivered boron to cells in all phases of the cell cycle, including S-phase. In vivo SIMS studies using the F98 rat glioma model revealed an 8:1 boron partitioning ratio between the main tumor mass and normal brain tissue with a 5:1 ratio between infiltrating tumor cells and contiguous normal brain. Since cis-ABCPC is water soluble and can cross the blood-brain-barrier via the L-type amino acid transporters (LAT, it may accumulate preferentially in infiltrating tumor cells in normal brain due to up-regulation of LAT in high grade gliomas. Once trapped inside the tumor cell, cis-ABCPC cannot be metabolized and remains either in a free pool or bound to cell matrix components. The significant improvement in boron uptake by both the main tumor mass and infiltrating tumor cells compared to those reported in animal and clinical studies of p-boronophenylalanine strongly suggest that cis-ABCPC has the potential to become a novel new boron delivery agent for neutron capture therapy of gliomas and melanomas.

  12. A quantitative extraction method for the determination of trace amounts of both butyl- and phenyltin compounds in sediments by gas chromatography-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Rajendran, R B; Tao, H; Nakazato, T; Miyazaki, A

    2000-10-01

    A simple and reliable extraction method was developed for quantitative determination of both butyl- and phenyltin compounds in sediments by capillary gas chromatography combined with inductively coupled plasma mass spectrometry (GC-ICP-MS). Both types of organotin compounds were extracted quantitatively from sediment by mechanical shaking into tropolone-toluene and HCl-methanol. After phase separation and pH adjustment, these organotins were ethylated with sodium tetraethylborate. The method was evaluated by analyzing PACS-2 and NIES No. 12 sediment certified reference materials. The dibutyltin (DBT; 1.14 +/- 0.02 micrograms g-1) and tributyltin (TBT; 1.01 +/- 0.04 micrograms g-1) values observed in PACS-2 sediment closely matched the certified values (DBT, 1.09 +/- 0.15; TBT, 0.98 +/- 0.13 microgram g-1 as tin). The monobutyltin (MBT) value was higher (0.62 +/- 0.02 microgram g-1) by more than two fold over the reference value (0.3 microgram g-1 as tin). The concentrations of TBT (0.18 +/- 0.04 microgram g-1) and triphenyltin (TPhT; 0.0099 +/- 0.002 microgram g-1) in the NIES No. 12 sediment were also in good agreement with the certified and reference values of TBT (0.19 +/- 0.03 microgram g-1 as compound) and TPhT (0.008 microgram g-1 as compound), respectively. Recoveries of TBT, tripentyltin (TPeT) and TPhT from spiked sediments were satisfactory (TBT, 102 +/- 3.4%; TPrT, 96 +/- 3.4%; TPhT, 99 +/- 8.5%). The detection limits as tin were in the range 0.23-0.48 ng g-1 for a 0.5 g sample size. It is also noteworthy that clean-up of the extract is not necessary because of the superior selectivity of ICP-MS detection. The present method was successfully applied to marine sediment samples. PMID:11070544

  13. Determination of volatile organic compounds in water by headspace solid-phase microextraction gas chromatography coupled to tandem mass spectrometry with triple quadrupole analyzer

    International Nuclear Information System (INIS)

    Highlights: → Employing a statistical optimization improves results reducing experiments. → Use of MS (QqQ) allows high sensitivity determination and improves identification capabilities. → Using Q/q intensity ratios is a powerful tool to ensure compound identification. → HS SPME GC-MS/MS method allows determination of VOCs in complex matrix water samples. - Abstract: In the present work, a rapid method with little sample handling has been developed for determination of 23 selected volatile organic compounds in environmental and wastewater samples. The method is based on headspace solid-phase microextraction (SPME) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) determination using triple quadrupole analyzer (QqQ) in electron ionization mode. The best conditions for extraction were optimised with a factorial design taking into account the interaction between different parameters and not only individual effects of variables. In the optimized procedure, 4 mL of water sample were extracted using a 10 mL vial and adding 0.4 g NaCl (final NaCl content of 10%). An SPME extraction with carboxen/polydimethylsiloxane 75 μm fiber for 30 min at 50 deg. C (with 5 min of previous equilibration time) with magnetic stirring was applied. Chromatographic determination was carried out by GC-MS/MS working in Selected Reaction Monitoring (SRM) mode. For most analytes, two MS/MS transitions were acquired, although for a few compounds it was difficult to obtain characteristic abundant fragments. In those cases, a pseudo selected reaction monitoring (pseudo-SRM) with three ions was used instead. The intensity ratio between quantitation (Q) and confirmation (q) signals was used as a confirmatory parameter. The method was validated by means of recovery experiments (n = 6) spiking mineral water samples at three concentration levels (0.1, 5 and 50 μg L-1). Recoveries between 70% and 120% were generally obtained with relative standard deviations (RSDs

  14. Determination of volatile organic compounds in water by headspace solid-phase microextraction gas chromatography coupled to tandem mass spectrometry with triple quadrupole analyzer

    Energy Technology Data Exchange (ETDEWEB)

    Cervera, M.I. [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain); Beltran, J., E-mail: joaquim.beltran@uji.es [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain); Lopez, F.J.; Hernandez, F. [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain)

    2011-10-17

    Highlights: {yields} Employing a statistical optimization improves results reducing experiments. {yields} Use of MS (QqQ) allows high sensitivity determination and improves identification capabilities. {yields} Using Q/q intensity ratios is a powerful tool to ensure compound identification. {yields} HS SPME GC-MS/MS method allows determination of VOCs in complex matrix water samples. - Abstract: In the present work, a rapid method with little sample handling has been developed for determination of 23 selected volatile organic compounds in environmental and wastewater samples. The method is based on headspace solid-phase microextraction (SPME) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) determination using triple quadrupole analyzer (QqQ) in electron ionization mode. The best conditions for extraction were optimised with a factorial design taking into account the interaction between different parameters and not only individual effects of variables. In the optimized procedure, 4 mL of water sample were extracted using a 10 mL vial and adding 0.4 g NaCl (final NaCl content of 10%). An SPME extraction with carboxen/polydimethylsiloxane 75 {mu}m fiber for 30 min at 50 deg. C (with 5 min of previous equilibration time) with magnetic stirring was applied. Chromatographic determination was carried out by GC-MS/MS working in Selected Reaction Monitoring (SRM) mode. For most analytes, two MS/MS transitions were acquired, although for a few compounds it was difficult to obtain characteristic abundant fragments. In those cases, a pseudo selected reaction monitoring (pseudo-SRM) with three ions was used instead. The intensity ratio between quantitation (Q) and confirmation (q) signals was used as a confirmatory parameter. The method was validated by means of recovery experiments (n = 6) spiking mineral water samples at three concentration levels (0.1, 5 and 50 {mu}g L{sup -1}). Recoveries between 70% and 120% were generally obtained with

  15. Application of high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS) for determination of chromium compounds in the air at the workplace.

    Science.gov (United States)

    Stanislawska, Magdalena; Janasik, Beata; Wasowicz, Wojciech

    2013-12-15

    The toxicity and bioavailability of chromium species are highly dependable on the form or species, therefore determination of total chromium is insufficient for a complete toxicological evaluation and risk assessment. An analytical method for determination of soluble and insoluble Cr (III) and Cr (VI) compounds in welding fume at workplace air has been developed. The total chromium (Cr) was determined by using quadruple inductively coupled plasma mass spectrometry (ICP-MS) equipped with a dynamic reaction cell (DRC(®)). Soluble trivalent and hexavalent chromium compounds were determined by high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS). A high-speed, reversed-phase CR C8 column (PerkinElmer, Inc., Shelton, CT, USA) was used for the speciation of soluble Cr (III) and soluble Cr (VI). The separation was accomplished by interaction of the chromium species with the different components of the mobile phase. Cr (III) formed a complex with EDTA, i.e. retained on the column, while Cr (VI) existed in the solutions as dichromate. Alkaline extraction (2% KOH and 3% Na2CO3) and anion exchange column (PRP-X100, PEEK, Hamilton) were used for the separation of the total Cr (VI). The results of the determination of Cr (VI) were confirmed by the analysis of the certified reference material BCR CRM 545 (Cr (VI) in welding dust). The results obtained for the certified material (40.2±0.6 g kg(-1)) and the values recorded in the examined samples (40.7±0.6 g kg(-1)) were highly consistent. This analytical method was applied for the determination of chromium in the samples in the workplace air collected onto glass (Whatman, Ø 37 mm) and membrane filters (Sartorius, 0.8 μm, Ø 37 mm). High performance liquid chromatography with inductively coupled plasma mass spectrometry is a remarkably powerful and versatile technique for determination of chromium species in welding fume at workplace air. PMID:24209303

  16. Neutron Capture Reactions for Stockpile Stewardship and Basic Science

    Energy Technology Data Exchange (ETDEWEB)

    Parker, W; Agvaanluvsan, U; Becker, J; Wilk, P; Wu, C; Bredeweg, T; Couture, A; Haight, R; Jandel, M; O' Donnell, J; Reifarth, R; Rundberg, R; Ullmann, J; Vieira, D; Wouters, J; Sheets, S; Mitchell, G; Becvar, F; Krticka, M

    2007-08-04

    The capture process is a nuclear reaction in which a target atom captures an incident projectile, e.g. a neutron. The excited-state compound nucleus de-excites by emitting photons. This process creates an atom that has one more neutron than the target atom, so it is a different isotope of the same element. With low energy (slow) neutron projectiles, capture is the dominant reaction, other than elastic scattering. However, with very heavy nuclei, fission competes with capture as a method of de-excitation of the compound nucleus. With higher energy (faster) incident neutrons, additional reactions are also possible, such as emission of protons or emission of multiple neutrons. The probability of a particular reaction occurring (such as capture) is referred to as the cross section for that reaction. Cross sections are very dependent on the incoming neutron's energy. Capture reactions can be studied either using monoenergetic neutron sources or 'white' neutron sources. A 'white' neutron source has a wide range of neutron energies in one neutron beam. The advantage to the white neutron source is that it allows the study of cross sections as they depend on neutron energies. The Los Alamos Neutron Science Center, located at Los Alamos National Laboratory, provides an intense white neutron source. Neutrons there are created by a high-energy proton beam from a linear accelerator striking a heavy metal (tungsten) target. The neutrons range in energy from subthermal up to very fast - over 100 MeV in energy. Low-energy neutron reaction cross sections fluctuate dramatically from one target to another, and they are very difficult to predict by theoretical modeling. The cross sections for particular capture reactions are important for defense sciences, advanced reactor concepts, transmutation of radioactive wastes and nuclear astrophysics. We now have a strong collaboration between Lawrence Livermore National Laboratory, Los Alamos National Laboratory

  17. Advances in mass spectrometric characterization of naphthenic acids fraction compounds in oil sands environmental samples and crude oil--A review.

    Science.gov (United States)

    Headley, John V; Peru, Kerry M; Barrow, Mark P

    2016-01-01

    There has been a recent surge in the development of mass spectrometric methods for detailed characterization of naphthenic acid fraction compounds (all C(c)H(h)N(n)O(o)S(s), species, including heteroatomic and aromatic components in the acid-extractable fraction) in environmental samples. This surge is driven by the increased activity in oil sands environmental monitoring programs in Canada, the exponential increase in research studies on the isolation and toxicity identification of components in oil sands process water (OSPW), and the analytical requirements for development of technologies for treatment of OSPW. There has been additional impetus due to the parallel studies to control corrosion from naphthenic acids during the mining and refining of heavy bitumen and crude oils. As a result, a range of new mass spectrometry tools have been introduced since our last major review of this topic in 2009. Of particular significance are the developments of combined mass spectrometric methods that incorporate technologies such as gas chromatography, liquid chromatography, and ion mobility. There has been additional progress with respect to improved visualization methods for petroleomics and oil sands environmental forensics. For comprehensive coverage and more reliable characterization of samples, an approach based on multiple-methods that employ two or more ionization modes is recommended. On-line or off-line fractionation of isolated extracts, with or without derivatization, might also be used prior to mass spectrometric analyses. Individual ionization methods have their associated strengths and weaknesses, including biases, and thus dependence upon a single ionization method is potentially misleading. There is also a growing trend to not rely solely on low-resolution mass spectrometric methods (power at m/z 200) for characterization of complex samples. Future research is anticipated to focus upon (i) structural elucidation of components to determine the correlation

  18. Encapsulated liquid sorbents for carbon dioxide capture

    Science.gov (United States)

    Vericella, John J.; Baker, Sarah E.; Stolaroff, Joshuah K.; Duoss, Eric B.; Hardin, James O.; Lewicki, James; Glogowski, Elizabeth; Floyd, William C.; Valdez, Carlos A.; Smith, William L.; Satcher, Joe H.; Bourcier, William L.; Spadaccini, Christopher M.; Lewis, Jennifer A.; Aines, Roger D.

    2015-02-01

    Drawbacks of current carbon dioxide capture methods include corrosivity, evaporative losses and fouling. Separating the capture solvent from infrastructure and effluent gases via microencapsulation provides possible solutions to these issues. Here we report carbon capture materials that may enable low-cost and energy-efficient capture of carbon dioxide from flue gas. Polymer microcapsules composed of liquid carbonate cores and highly permeable silicone shells are produced by microfluidic assembly. This motif couples the capacity and selectivity of liquid sorbents with high surface area to facilitate rapid and controlled carbon dioxide uptake and release over repeated cycles. While mass transport across the capsule shell is slightly lower relative to neat liquid sorbents, the surface area enhancement gained via encapsulation provides an order-of-magnitude increase in carbon dioxide absorption rates for a given sorbent mass. The microcapsules are stable under typical industrial operating conditions and may be used in supported packing and fluidized beds for large-scale carbon capture.

  19. CHAOTIC CAPTURE OF NEPTUNE TROJANS

    International Nuclear Information System (INIS)

    Neptune Trojans (NTs) are swarms of outer solar system objects that lead/trail planet Neptune during its revolutions around the Sun. Observations indicate that NTs form a thick cloud of objects with a population perhaps ∼10 times more numerous than that of Jupiter Trojans and orbital inclinations reaching ∼25 deg. The high inclinations of NTs are indicative of capture instead of in situ formation. Here we study a model in which NTs were captured by Neptune during planetary migration when secondary resonances associated with the mean-motion commensurabilities between Uranus and Neptune swept over Neptune's Lagrangian points. This process, known as chaotic capture, is similar to that previously proposed to explain the origin of Jupiter's Trojans. We show that chaotic capture of planetesimals from an ∼35 Earth-mass planetesimal disk can produce a population of NTs that is at least comparable in number to that inferred from current observations. The large orbital inclinations of NTs are a natural outcome of chaotic capture. To obtain the ∼4:1 ratio between high- and low-inclination populations suggested by observations, planetary migration into a dynamically excited planetesimal disk may be required. The required stirring could have been induced by Pluto-sized and larger objects that have formed in the disk.

  20. Comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry for the forensic study of cadaveric volatile organic compounds released in soil by buried decaying pig carcasses.

    Science.gov (United States)

    Brasseur, Catherine; Dekeirsschieter, Jessica; Schotsmans, Eline M J; de Koning, Sjaak; Wilson, Andrew S; Haubruge, Eric; Focant, Jean-Francois

    2012-09-14

    This article reports on the use of comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS) for forensic geotaphonomy application. Gravesoil samples were collected at various depths and analyzed for their volatile organic compound (VOC) profile. A data processing procedure was developed to highlight potential candidate marker molecules related to the decomposition process that could be isolated from the soil matrix. Some 20 specific compounds were specifically found in the soil sample taken below the carcass and 34 other compounds were found at all depths of the gravesoil samples. The group of the 20 compounds consisted of ketones, nitriles, sulfurs, heterocyclic compounds, and benzene derivatives like aldehydes, alcohols, ketones, ethers and nitriles. The group of the 34 compounds consisted of methyl-branched alkane isomers including methyl-, dimethyl-, trimethyl-, tetramethyl-, and heptamethyl-isomers ranging from C(12) to C(16). A trend in the relative presence of these alkanes over the various layers of soils was observed, with an increase in the amount of the specific alkanes when coming from the carcass to the surface. Based on the specific presence of these methyl-branched alkanes in gravesoils, we created a processing method that applies a specific script to search raw data for characteristic mass spectral features related to recognizable mass fragmentation pattern. Such screening of soil samples for cadaveric decomposition signature was successfully applied on two gravesoil sites and clearly differentiates soils at proximity of buried decaying pig carcasses from control soils. PMID:22520639

  1. Video Screen Capture Basics

    Science.gov (United States)

    Dunbar, Laura

    2014-01-01

    This article is an introduction to video screen capture. Basic information of two software programs, QuickTime for Mac and BlueBerry Flashback Express for PC, are also discussed. Practical applications for video screen capture are given.

  2. Molecularly imprinted solid phase extraction using stable isotope labeled compounds as template and liquid chromatography-mass spectrometry for trace analysis of bisphenol A in water sample

    International Nuclear Information System (INIS)

    We have developed a molecularly imprinted polymer (MIP) using a stable isotope labeled compound as the template molecule and called it the ''isotope molecularly imprinted polymer'' (IMIP). In this study, bisphenol A (BPA) was used as the model compound. None imprinted polymer (NIP), MIP, dummy molecularly imprinted polymer (DMIP) and IMIP were prepared by the suspension polymerization method using without template, BPA, 4-tert-butylphenol (BP) and bisphenol A-d16 (BPA-d16), respectively. The polymers were subjected to molecularly imprinted solid phase extraction (MI-SPE), and the extracted samples were subjected to liquid chromatography-mass spectrometry (LC-MS). Although the leakage of BPA-d16 from the IMIP was observed and that of BPA was not observed. The selectivity factors of MIP and IMIP for BPA were 4.45 and 4.43, respectively. Therefore, IMIP had the same molecular recognition ability as MIP. When MI-SPE with IMIP was used and followed by LC-MS in the analysis of river water sample, the detection limit of BPA was 1 ppt with high sensitivity. Moreover, the average recovery was higher than 99.8% (R.S.D.: 3.7%) by using bisphenol A-13C12 (BPA-13C12) as the surrogate standard. In addition, the IMIP were employed in MI-SPE of BPA in river water sample by LC-MS. The concentration of BPA in the river water sample was determined to be 32 pg ml-1. We confirmed that it was possible to measure trace amounts of a target analyte by MI-SPE using IMIP

  3. Fluorocarbon-bonded magnetic mesoporous microspheres for the analysis of perfluorinated compounds in human serum by high-performance liquid chromatography coupled to tandem mass spectrometry

    International Nuclear Information System (INIS)

    Highlights: • New SPE method was developed for analysis of PFCs in human serum. • Fluorocarbon-bonded magnetic mesoporous microspheres were used as SPE absorbents. • PFCs in serum were directly extracted without any other pretreatment procedure. • The PFCs-adsorbed microspheres were simply and rapidly isolated by using a magnet. - Abstract: We report herein an extraction method for the analysis of perfluorinated compounds in human serum based on magnetic core–mesoporous shell microspheres with decyl-perfluorinated interior pore-walls (Fe3O4@mSiO2-F17). Thanks to the unique properties of the Fe3O4@mSiO2-F17 microspheres, macromolecules like proteins could be easily excluded from the mesoporous channels due to size exclusion effect, and perfluorinated compounds (PFCs) in protein-rich biosamples such as serum could thus be directly extracted with the fluorocarbon modified on the channel wall without any other pretreatment procedure. The PFCs adsorbed Fe3O4@mSiO2-F17 microspheres could then be simply and rapidly isolated by using a magnet, followed by being identified and quantified by LC–MS/MS (high-performance liquid chromatography coupled to tandem mass spectrometry). Five perfluorinatedcarboxylic acids (C6, C8–C11) and perfluorooctane sulfonate (PFOS) were selected as model analytes. In order to achieve the best extraction efficiency, some important factors including the amount of Fe3O4@mSiO2-F17 microspheres added, adsorption time, type of elution solvent, eluting solvent volume and elution time were investigated. The ranges of the LOD were 0.02–0.05 ng mL−1 for the six PFCs. The recovery of the optimized method varies from 83.13% to 92.42% for human serum samples

  4. Waveform Catalog, Extreme Mass Ratio Binary (Capture)

    Data.gov (United States)

    National Aeronautics and Space Administration — Numerically-generated gravitational waveforms for circular inspiral into Kerr black holes. These waveforms were developed using Scott Hughes' black hole...

  5. Collision energy dependence of He and Ne capture by C sup + sub 60

    Energy Technology Data Exchange (ETDEWEB)

    Campbell, E.E.B.; Ehlich, R.; Hielscher, A.; Frazao, J.M.A.; Hertel, I.V. (Freiburg Univ. (Germany). Fakultaet fuer Physik Freiburg Univ. (Germany). Freiburger Materialforschungszentrum (FMF))

    1992-04-01

    Recently, reports of the formation of endohedral cluster compounds He{alpha}C{sup +}{sub n} and Ne{alpha}C{sup +}{sub n-4} (n even and {<=}60) have been published for high energy collisions between C{sup +}{sub 60} and rare gases. Here we present the collision energy dependence for the formation of He{alpha}C{sup +}{sub 60} and Ne{alpha}C{sup +}{sub 60} in the region of the energetic threshold for the capture process. The threshold for He capture lies at 6{+-}2 eV in the centre of mass reference frame whereas that for Ne lies somewhat higher at 9{+-}1 eV. ({alpha} means endohedral fulleren compounds.) (orig.).

  6. Enhancement of sensitivity in the determination of organic trace compounds in complex matrices with liquid chromatography-mass spectrometry (LC-MS)

    International Nuclear Information System (INIS)

    The PhD-thesis deals with 'enhancement of sensitivity in the determination of organic trace compounds in complex matrices with liquid chromatography-mass spectrometry (LC-MS)'. Almost the most important factor is the enhancement of the ionization yield with Atmospheric Pressure Chemical Ionization (APCI) or Electrospray Ionization (ESI) in LC-MS. Ionization yields of different compounds can vary by a factor of 10000. Three ways to solve this problem of little ionization yield were tried: 1) Modification of the mobile phase in HPLC 2) Chemical modification of the analytes 3) A new type of ionization called Atmospheric Pressure Photo Ionization (APPI). ad 1) By using specific additives to mobile phases ion suppression that might derive from an ion pair reagent that was necessary for chromatography could be omitted. General remarks cannot be done. ad 2) Chemical modification or so called derivatization is well known for UV- and fluorescence-detection for a long period of time. As substances containing nitrogene (e.g. primary, secondary or tertiary amines) often have good ionization yields, poor or relatively poor ionizable substances like carboxylic acids, sugars and partially phenolic steroids were used as analytes for derivatization reactions. By using Dansyl as Dansylchlorid or Dansylhydrazine a basic derivatization agent could be found that ionizes very well. A 200 times more sensitive determination of estrogenes is possible after derivatization with Dansylchlorid. Using a tandem-mass-spectrometer a lower limit of quantification of 2 pg/mL plasma could be reached by using 1 mL of plasma. For ketones like carvon and campher an enhancement by a factor of 500 and 4000 could be reached by using Dansylhydrazine as the derivatization agent. For fatty acids DMEQ as derivatization agent enhanced the sensitivity by a factor of 20 to 100. ad 3) APPI as a new ionization mode showed really good results for specific molecules. Relatively unpolar substances as diphenylsulfide

  7. Radiative electron capture

    International Nuclear Information System (INIS)

    Some data are presented for radiative electron capture by fast moving ions. The radiative electron capture spectrum is shown for O8+ in Ag, along with the energy dependence of the capture cross-section. A discrepancy between earlier data, theoretical prediction, and the present data is pointed out. (3 figs) (U.S.)

  8. X-231A demonstration of in-situ remediation of DNAPL compounds in low permeability media by soil fracturing with thermally enhanced mass recovery or reactive barrier destruction

    International Nuclear Information System (INIS)

    The overall goal of the program of activities is to demonstrate robust and cost-effective technologies for in situ remediation of DNAPL compounds in low permeability media (LPM), including adaptations and enhancements of conventional technologies to achieve improved performance for DNAPLs in LPM. The technologies sought should be potential for application at simple, small sites (e.g., gasoline underground storage tanks) as well as at complex, larger sites (e.g., DOE land treatment units). The technologies involved in the X-231A demonstration at Portsmouth Gaseous Diffusion Plant (PORTS) utilized subsurface manipulation of the LPM through soil fracturing with thermally enhanced mass recovery or horizontal barrier in place destruction. To enable field evaluation of these approaches, a set of four test cells was established at the X-231A land treatment unit at the DOE PORTS plant in August 1996 and a series of demonstration field activities occurred through December 1997. The principal objectives of the PORTS X-231A demonstration were to: determine and compare the operational features of hydraulic fractures as an enabling technology for steam and hot air enhanced soil vapor extraction and mass recovery, in situ interception and reductive destruction by zero valent iron, and in situ interception and oxidative destruction by potassium permanganate; determine the interaction of the delivered agents with the LPM matrix adjacent to the fracture and within the fractured zone and assess the beneficial modifications to the transport and/or reaction properties of the LPM deposit; and determine the remediation efficiency achieved by each of the technology strategies

  9. Antioxidant activity and identification of bioactive compounds from leaves of Anthocephalus cadamba by ultra-performance liquid chromatography/electrospray ionization quadrupole time of flight mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    Madhu Chandel; Upendra Sharma; Neeraj Kumar; Bikram Singh; Satwinderjeet Kaur

    2012-01-01

    Objective: To evaluate the antioxidant potential of different extract/fractions of Anthocephalus cadamba (A. cadamba) (Roxb.) Miq. (Rubiaceae) and study the tentative identification of their active constituents. Methods: The extract/fractions were screened for antioxidant activity using various in vitro assays viz. DPPH assay, ABTS assay, superoxide anion radical scavenging assay, reducing power assay and plasmid DNA nicking assay. Total phenolic content of extract/fractions was determined by colorimetric method. An ultra-performance LC-electrospray-quadrupole-time of flight mass spectrometry method was used to analyse the active constituents of extract/fractions of A. cadamba. Results: The ethyl acetate fraction was found to be most active fraction in all the assays as compared to other extract/fractions. The IC50 value of ethyl acetate fraction (ETAC fraction) was 21.24 μg/mL, 1.12 μg/mL, 9.68 μg/mL and 57.81 μg/mL in DPPH assay, ABTS assay, reducing power assay and superoxide scavenging assay respectively. All the extract/fractions also showed the potential to protect the plasmid DNA (pBR322) against the attack of hydroxyl radicals generated by Fenton’s reagent. The bioactive compounds were identified by UPLC-ESI-QTOF-MS, by comparing the mass and λmax with literature values. Conclusions: The potential of the extract/fractions to scavenge different free radicals in different systems indicated that they may be useful therapeutic agents for treating radical-related pathologic damage.

  10. X-231A demonstration of in-situ remediation of DNAPL compounds in low permeability media by soil fracturing with thermally enhanced mass recovery or reactive barrier destruction

    Energy Technology Data Exchange (ETDEWEB)

    Siegrist, R.L. [Oak Ridge National Lab., TN (United States)]|[Colorado School of Mines, Golden, CO (United States). Environmental Science and Engineering Div.; Lowe, K.S. [Oak Ridge National Lab., Grand Junction, CO (United States). Life Sciences Div.; Murdoch, L.D. [FRx, Inc., Cincinnati, OH (United States)]|[Clemson Univ., SC (United States); Slack, W.W. [FRx, Inc., Cincinnati, OH (United States); Houk, T.C. [Lockheed Martin Energy Systems, Piketon, OH (United States)

    1998-03-01

    The overall goal of the program of activities is to demonstrate robust and cost-effective technologies for in situ remediation of DNAPL compounds in low permeability media (LPM), including adaptations and enhancements of conventional technologies to achieve improved performance for DNAPLs in LPM. The technologies sought should be potential for application at simple, small sites (e.g., gasoline underground storage tanks) as well as at complex, larger sites (e.g., DOE land treatment units). The technologies involved in the X-231A demonstration at Portsmouth Gaseous Diffusion Plant (PORTS) utilized subsurface manipulation of the LPM through soil fracturing with thermally enhanced mass recovery or horizontal barrier in place destruction. To enable field evaluation of these approaches, a set of four test cells was established at the X-231A land treatment unit at the DOE PORTS plant in August 1996 and a series of demonstration field activities occurred through December 1997. The principal objectives of the PORTS X-231A demonstration were to: determine and compare the operational features of hydraulic fractures as an enabling technology for steam and hot air enhanced soil vapor extraction and mass recovery, in situ interception and reductive destruction by zero valent iron, and in situ interception and oxidative destruction by potassium permanganate; determine the interaction of the delivered agents with the LPM matrix adjacent to the fracture and within the fractured zone and assess the beneficial modifications to the transport and/or reaction properties of the LPM deposit; and determine the remediation efficiency achieved by each of the technology strategies.

  11. Theoretical neutron-capture cross sections for r-process nucleosynthesis in the $^{48}$Ca region

    CERN Document Server

    Rauscher, T; Kratz, K -L; Balogh, W; Oberhummer, H

    2015-01-01

    We calculate neutron capture cross sections for r-process nucleosynthesis in the $^{48}$Ca region, namely for the isotopes $^{40-44}$S, $^{46-50}$Ar, $^{56-66}$Ti, $^{62-68}$Cr, and $^{72-76}$Fe. While previously only cross sections resulting from the compound nucleus reaction mechanism (Hauser-Feshbach) have been considered, we recalculate not only that contribution to the cross section but also include direct capture on even-even nuclei. The level schemes, which are of utmost importance in the direct capture calculations, are taken from quasi-particle states obtained with a folded-Yukawa potential and Lipkin-Nogami pairing. Most recent deformation values derived from experimental data on $\\beta$-decay half lives are used where available. Due to the consideration of direct capture, the capture rates are enhanced and the "turning points" in the r-process path are shifted to slightly higher mass numbers. We also discuss the sensitivity of the direct capture cross sections on the assumed deformation.

  12. Capture Their Attention: Capturing Lessons Using Screen Capture Software

    Science.gov (United States)

    Drumheller, Kristina; Lawler, Gregg

    2011-01-01

    When students miss classes for university activities such as athletic and academic events, they inevitably miss important class material. Students can get notes from their peers or visit professors to find out what they missed, but when students miss new and challenging material these steps are sometimes not enough. Screen capture and recording…

  13. Linear and mass attenuation coefficient for CdTe compound of X-rays from 10 to 100 keV energy range in different phases

    International Nuclear Information System (INIS)

    The Full Potential Linear Muffin Tin Orbitals method within the density functional theory has been utilized to calculate structural and electronic properties of the CdTe compound. We have checked that the CdTe has two phase-transitions from zinc-blend to cinnabar and from cinnabar to rocksalt. We have found that the rigidity, the energy and the nature of the gap change according to the phase change, so we can predict that a CdTe detector may have different behaviors in different phase conditions. In order to investigate this behavior change, the linear and the mass attenuation coefficients of X-ray in rocksalt, zinc-blend and cinnabar structures are calculated from 10 keV to100 keV, using the XCOM data. We have found that when CdTe undergoes a phase transition from zinc-blend to cinnabar, its linear attenuation coefficient decreases down to a value of about 100 times smaller than its initial one, and when it undergoes a transition from cinnabar to rocksalt it increases up to a value about 90 times larger than its initial one

  14. Nano-speciation in solution of radionuclides by electro-spray mass spectrometry and prospectives for the speciation on solid of organic and organometallic compounds

    International Nuclear Information System (INIS)

    The speciation of radionuclides in presence of multiple ligands in complex matrices in the industrial fields (reactor, reprocessing...), environmental, biological is a main challenge to better understand their behaviour. Among the speciation techniques, the electro-spray mass spectrometry (ES-MS) allows to study the radionuclides, the ligand and the complexes associated to the covalent/non covalent interactions of radionuclides - ligand. Advances in the ionization source allow to work now with a rate 100 time inferior to the classical ES-MS with a better sensitivity and in improving the speciation capacities. Recent results obtained on radionuclides nano-speciation by ES-MS with correlation by temporal resolution laser spectro-fluorimetry have especially allowed the obtention of complexation constants. The nuclearization of an ES-MS source with nano-ionization and the prospectives of the Direct Analysis in Real Time and Desorption Electro-spray Source Ionization sources for the direct speciation of organic and organometallic compounds chemisorbed/grafted on surface will be approached. (O.M.)

  15. Impact of gas chromatography and mass spectrometry combined with gas chromatography and olfactometry for the sex differentiation of Baccharis articulata by the analysis of volatile compounds.

    Science.gov (United States)

    Minteguiaga, Manuel; Umpiérrez, Noelia; Fariña, Laura; Falcão, Manuel A; Xavier, Vanessa B; Cassel, Eduardo; Dellacassa, Eduardo

    2015-09-01

    The Baccharis genus has more than 400 species of aromatic plants. However, only approximately 50 species have been studied in oil composition to date. From these studies, very few take into consideration differences between male and female plants, which is a significant and distinctive factor in Baccharis in the Asteraceae family. Baccharis articulata is a common shrub that grows wild in south Brazil, northern and central Argentina, Bolivia, Paraguay and Uruguay. It is considered to be a medicinal plant and is employed in traditional medicine. We report B. articulata male and female volatile composition obtained by simultaneous distillation-extraction technique and analyzed by gas chromatography with mass spectrometry. Also, an assessment of aromatic differences between volatile extracts was evaluated by gas chromatography with olfactometry. The results show a very similar chemical composition between male and female extracts, with a high proportion of terpene compounds of which β-pinene, limonene and germacrene D are the main components. Despite the chemical similarity, great differences in aromatic profile were found: male plant samples exhibited the strongest odorants in number and intensity of aromatic attributes. These differences explain field observations which indicate differences between male and female flower aroma, and might be of ecological significance in the attraction of pollinating insects. PMID:26140379

  16. Using electrospray-assisted laser desorption/ionization mass spectrometry to characterize organic compounds separated on thin-layer chromatography plates.

    Science.gov (United States)

    Lin, Shu-Yao; Huang, Min-Zong; Chang, Hui-Chiu; Shiea, Jentaie

    2007-11-15

    Electrospray-assisted laser desorption/ionization (ELDI), an ionization method that combines laser desorption and electrospray ionization (ESI), can be used under ambient conditions to characterize organic compounds (including FD&C dyes, amines, extracts of a drug tablet) separated in the central track on a thin-layer chromatography (TLC) plate coated with either reversed-phase C18 particles or normal-phase silica gel. After drying, the TLC plate was placed on an acrylic sample holder set in front of the sampling skimmer of an ion trap mass analyzer. The chemicals at the center of the TLC plate were analyzed by pushing the sample holder into the path of a laser beam with a syringe pump. The molecules in the sample spot were desorbed by continuously irradiating the surface of the TLC plate with a pulsed nitrogen laser. Then, the desorbed sample molecules entered an ESI plume where they were ionized through the reactions with the charged species (including protons, hydronium ions and their cluster ions, solvent ions, and charged droplets) generated by electrospraying a methanol/water solution. MS/MS analyses were also performed to further characterize the analytes. The detection limit of TLC/ELDI/MS is approximately 10(-6) M. This was evaluated by using FD&C red dye as the standard. A linear relationship was found for the calibration curve with the concentration of FD&C red dye ranged from 10(-3) to 10(-6) M. PMID:17929897

  17. Stir frit microextraction: an approach for the determination of volatile compounds in water by headspace-gas chromatography/mass spectrometry.

    Science.gov (United States)

    Roldán-Pijuán, M; Alcudia-León, M C; Lucena, R; Cárdenas, S; Valcárcel, M

    2012-08-17

    In this article, a novel extraction approach, called stir frit microextraction (SFME), is presented. The new approach combines the extractive capability of a commercial polyethylene frit (20 μm of pore size) with the stirring in the same device. The proposed extraction procedure allows the determination of benzene, toluene, ethylbenzene, xylene isomers and styrene (BTEX-S) in water samples. The analytes are extracted on the frit, previously conditioned with methanol, under continuous magnetic stirring. Once the extraction is performed, the frit is transferred to a headspace vial where the volatile compounds are desorbed from the frit (90 °C, 30 min) in a headspace module and analyzed by gas chromatography/mass spectrometry. Headspace conditions (time and temperature) as well as extraction conditions (ionic strength, type of stirring, extraction time, stirring rate and sample volume) have been systematically evaluated. The method was characterized on the basis of its linearity, sensitivity and precision. Limits of detection were in the range from 18 ng/L (o-xylene) to 65 ng/L (benzene). The repeatability of the proposed method, expressed as relative standard deviation (RSD) varied between 3.8% (toluene) and 8.2% (m- and p-xylene). The recovery study carried out in different water samples provided an average recovery of 94%, which demonstrated the applicability of the stir frit microextraction for the analytical problem selected in this article. PMID:22771255

  18. Simultaneous monitoring of seven phenolic metabolites of endocrine disrupting compounds (EDC) in human urine using gas chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Schmidt, Lukas; Müller, Johannes; Göen, Thomas

    2013-02-01

    A gas chromatographic-tandem mass spectrometric (GC-MS/MS) method for the simultaneous determination of the three well-known endocrine disruptors, bisphenol A, daidzein and genistein, as well as of four human pesticide metabolites which are supposed to have proper endocrine activity or which are metabolites of endocrine-disrupting compounds, viz., 1- and 2-naphthol, 2-isopropoxyphenol and 3,5,6-trichloropyridinol, has been developed and validated. The method involves enzymatic cleavage of the conjugates using β-glucuronidase/arylsulfatase followed by solid-phase extraction and derivatisation with N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide. Isotopically labelled internal standards were used for all analytes, to achieve best analytical error correction. The method proved to be both sensitive and reliable in human urine with detection limits ranging from 0.1 to 0.6 μg/L for all analytes. Precision and repeatability was determined to range from 1 to 15 %. Compared with other published analytical procedures, the present method enables the simultaneous determination of a couple of phenolic agents with competitive or improved analytical reliability. Thus, the present method is suitable for a combined monitoring of the exposure to prominent xenobiotics with effects on the human endocrine system (bisphenol A, carbaryl, chlorpyrifos, chlorpyrifos-methyl, naphthalene, propoxur, triclopyr) and phytoestrogens (daidzein, genistein) in population studies. PMID:23241820

  19. Comparison of the Volatile Compounds among Different Production Regions of Green Tea using Simultaneous Distillation Extraction Coupled with Gas Chromatography-mass Spectrometry

    Directory of Open Access Journals (Sweden)

    J.S. Zhou

    2015-03-01

    Full Text Available Chinese green teas are mainly made of the leaves of the plant Camellia sinensis and mainly distributed in provinces of Zhejiang, Anhui, Henan and Jiangsu, etc. Because of having same tea varieties and processing technology, different origins of green teas are very similar in appearance. Whereas different production areas and climatic conditions between them may have cause different quality characters, such as aroma and taste. So it is very necessary to study the different regions of green teas and explore environment and geographical factors to volatile components influence. In this study, the aroma components of four typical green teas: Xihulongjing, Xinyangmaojian, Lu’anguapian and Biluochun, from Zhejiang, Henan, Anhui and Jiangsu in China, were extracted by Simultaneous Distillation Extraction (SDE and identified by Gas Chromatography-Mass Spectrometry (GC-MS, then compared the similarities and differences between them on the aroma components was made. The result showed that 61 aroma constituents were indentified in four green teas, mainly including alcohols, hydrocarbons and ketones compounds. Through contrast and comparison of results, we find that these different origins of green teas have some differences, but also share some similarities based on the volatile components. The difference of place of origin and elevation will grow different tea plants and will have different volatile components due to the environment.

  20. Linear and mass attenuation coefficient for CdTe compound of X-rays from 10 to 100 keV energy range in different phases

    Energy Technology Data Exchange (ETDEWEB)

    Saim, A., E-mail: saim1989asma@gmail.com; Tebboune, A.; Berkok, H.; Belameiri, N.; Belbachir, A.H.

    2014-07-25

    The Full Potential Linear Muffin Tin Orbitals method within the density functional theory has been utilized to calculate structural and electronic properties of the CdTe compound. We have checked that the CdTe has two phase-transitions from zinc-blend to cinnabar and from cinnabar to rocksalt. We have found that the rigidity, the energy and the nature of the gap change according to the phase change, so we can predict that a CdTe detector may have different behaviors in different phase conditions. In order to investigate this behavior change, the linear and the mass attenuation coefficients of X-ray in rocksalt, zinc-blend and cinnabar structures are calculated from 10 keV to100 keV, using the XCOM data. We have found that when CdTe undergoes a phase transition from zinc-blend to cinnabar, its linear attenuation coefficient decreases down to a value of about 100 times smaller than its initial one, and when it undergoes a transition from cinnabar to rocksalt it increases up to a value about 90 times larger than its initial one.

  1. The Electron Capture $^{163}$Ho Experiment ECHo

    CERN Document Server

    Blaum, K; Duellmann, C E; Eberhardt, K; Eliseev, S; Enss, C; Faessler, A; Fleischmann, A; Gastaldo, L; Kempf, S; Krivoruchenko, M; Lahiri, S; Maiti, M; Novikov, Yu N; Ranitzsch, P C -O; Simkovic, F; Szusc, Z; Wegner, M

    2013-01-01

    The determination of the absolute scale of the neutrino masses is one of the most challenging questions in particle physics. Different approaches are followed to achieve a sensitivity on neutrino masses in the sub-eV range. Among them, experiments exploring the beta decay and electron capture processes of suitable nuclides can provide necessary information on the electron neutrino mass value. In this talk we present the Electron Capture 163-Ho experiment ECHo, which aims to investigate the electron neutrino mass in the sub-eV range by means of the analysis of the calorimetrically measured energy spectrum following the electron capture process of 163-Ho. A high precision and high statistics spectrum will be measured by means of low temperature magnetic calorimeter arrays. We present preliminary results obtained with a first prototype of single channel detectors as well as the participating groups and their on-going developments.

  2. Quantitative evaluation of boron neutron capture therapy (BNCT) drugs for boron delivery and retention at subcellular scale resolution in human glioblastoma cells with imaging secondary ion mass spectrometry (SIMS)

    Science.gov (United States)

    Chandra, S.; Ahmad, T.; Barth, R. F.; Kabalka, G. W.

    2014-01-01

    Boron neutron capture therapy (BNCT) of cancer depends on the selective delivery of a sufficient number of boron-10 (10B) atoms to individual tumor cells. Cell killing results from the 10B (n, α)7Li neutron capture and fission reactions that occur if a sufficient number of 10B atoms are localized in the tumor cells. Intranuclear 10B localization enhances the efficiency of cell killing via damage to the DNA. The net cellular content of 10B atoms reflects both bound and free pools of boron in individual tumor cells. The assessment of these pools, delivered by a boron delivery agent, currently cannot be made at subcellular scale resolution by clinically applicable techniques such as PET and MRI. In this study, secondary ion mass spectrometry (SIMS) based imaging instrument, a CAMECA IMS 3f ion microscope, capable of 500 nm spatial resolution was employed. Cryogenically prepared cultured human T98G glioblastoma cells were evaluated for boron uptake and retention of two delivery agents. The first, L-p-boronophenylalanine (BPA), has been used clinically for BNCT of high grade gliomas, recurrent tumors of the head and neck region and melanomas. The second, a boron analogue of an unnatural amino acid, 1-amino-3-borono-cyclopentanecarboxylic acid (cis-ABCPC), has been studied in rodent glioma and melanoma models by quantification of boron in the nucleus and cytoplasm of individual tumor cells. The bound and free pools of boron were assessed by exposure of cells to boron-free nutrient medium. Both BPA and cis-ABCPC delivered almost 70% of the pool of boron in the free or loosely bound form to the nucleus and cytoplasm of human glioblastoma cells. This free pool of boron could be easily mobilized out of the cell and was in some sort of equilibrium with extracellular boron. In the case of BPA, the intracellular free pool of boron also was affected by the presence of phenylalanine in the nutrient medium. This suggests that it might be advantageous if patients were placed on a

  3. Applications of Solid-Phase Microextraction and Gas Chromatography/Mass Spectrometry (SPME-GC/MS) in the Study of Grape and Wine Volatile Compounds

    OpenAIRE

    Annarita Panighel; Riccardo Flamini

    2014-01-01

    Volatile compounds are responsible for the wine “bouquet”, which is perceived by sniffing the headspace of a glass, and of the aroma component (palate-aroma) of the overall flavor, which is perceived on drinking. Grape aroma compounds are transferred to the wine and undergo minimal alteration during fermentation (e.g., monoterpenes and methoxypyrazines); others are precursors of aroma compounds which form in winemaking and during wine aging (e.g., glycosidically-bound volatile compounds and C...

  4. Development of a hollow fibre liquid-phase micro extraction method coupled with capillary electrophoresis/mass spectrometry for determining nitrophenolic compounds from atmospheric particles

    Science.gov (United States)

    Teich, Monique; van Pinxteren, Dominik; Herrmann, Hartmut

    2014-05-01

    Nitrophenolic compounds present in the atmosphere gained a lot of attention as they are known for their negative effect on human health as well as for their phytotoxity being a cause for forest decline. Moreover, nitrophenols have the ability to absorb light in the range of near ultra violet to visible light, thus they are also contributing to the so-called brown carbon. Most of the available methods for determining nitrophenols in particulate matter are using organic solvents for extraction. Those methods are not applicable if one wants to focus only on the water-soluble fraction. Therefore, a method using a three-phase hollow fibre liquid-phase micro extraction (HF-LPME) was developed to enrich nine nitrophenolic compounds (2-Nitrophenol, 3-Nitrophenol, 4-Nitrophenol, 2-Methyl-4-nitrophenol, 3-Methyl-4-nitrophenol, 4-Nitrocatechol, 2,6-Dimethyl-4-nitrophenol, 2,4-Dinitrophenol, 3,4-Dinitrophenol) from aqueous extracts of atmospheric particles. Analysis was performed by capillary electrophoresis coupled with electrospray ionisation mass spectrometry (CE-ESI-MS). The background electrolyte composition was optimised to a 20 mM ammonium acetate buffer at pH 9.7 containing 15% methanol (v/v). Persistent peak tailing during electrophoretic separation was observed for 4-Nitrocatechol. Flushing the capillary with Ethylenediaminetetraacetic acid (EDTA) prior sample injection strongly improved the peak shape. Four extraction parameters (composition of organic liquid membrane, pH of acceptor phase, salting out effect, extraction time) and their effect on the analyte recoveries were examined. The HF-LPME consisted of 1.8 mL sample solution kept at pH 2 as donor phase and 15 µl 100 mM aqueous ammonia solution as acceptor phase inserted into a hollow fibre. Dihexyl ether was used to form a supported liquid membrane inside the pores of the hollow fibre. As a result low detection limits in the range of nmol L-1 were achieved and the developed method was found to be competitive

  5. A METHOD FOR AUTOMATED ANALYSIS OF 10 ML WATER SAMPLES CONTAINING ACIDIC, BASIC, AND NEUTRAL SEMIVOLATILE COMPOUNDS LISTED IN USEPA METHOD 8270 BY SOLID PHASE EXTRACTION COUPLED IN-LINE TO LARGE VOLUME INJECTION GAS CHROMATOGRAPHY/MASS SPECTROMETRY

    Science.gov (United States)

    Data is presented showing the progress made towards the development of a new automated system combining solid phase extraction (SPE) with gas chromatography/mass spectrometry for the single run analysis of water samples containing a broad range of acid, base and neutral compounds...

  6. Fluorocarbon-bonded magnetic mesoporous microspheres for the analysis of perfluorinated compounds in human serum by high-performance liquid chromatography coupled to tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Xiaodan; Yu, Yingjia [Department of Pharmaceutical Analysis, School of Pharmacy, Fudan University, No. 826 Zhangheng Road, Shanghai 201203 (China); Li, Yan, E-mail: yanli@fudan.edu.cn [Department of Pharmaceutical Analysis, School of Pharmacy, Fudan University, No. 826 Zhangheng Road, Shanghai 201203 (China); Zhang, Haiying [Department of Biology, Dezhou University, Shandong 253023 (China); Ling, Jin; Sun, Xueni; Feng, Jianan; Duan, Gengli [Department of Pharmaceutical Analysis, School of Pharmacy, Fudan University, No. 826 Zhangheng Road, Shanghai 201203 (China)

    2014-09-24

    Highlights: • New SPE method was developed for analysis of PFCs in human serum. • Fluorocarbon-bonded magnetic mesoporous microspheres were used as SPE absorbents. • PFCs in serum were directly extracted without any other pretreatment procedure. • The PFCs-adsorbed microspheres were simply and rapidly isolated by using a magnet. - Abstract: We report herein an extraction method for the analysis of perfluorinated compounds in human serum based on magnetic core–mesoporous shell microspheres with decyl-perfluorinated interior pore-walls (Fe{sub 3}O{sub 4}@mSiO{sub 2}-F{sub 17}). Thanks to the unique properties of the Fe{sub 3}O{sub 4}@mSiO{sub 2}-F{sub 17} microspheres, macromolecules like proteins could be easily excluded from the mesoporous channels due to size exclusion effect, and perfluorinated compounds (PFCs) in protein-rich biosamples such as serum could thus be directly extracted with the fluorocarbon modified on the channel wall without any other pretreatment procedure. The PFCs adsorbed Fe{sub 3}O{sub 4}@mSiO{sub 2}-F{sub 17} microspheres could then be simply and rapidly isolated by using a magnet, followed by being identified and quantified by LC–MS/MS (high-performance liquid chromatography coupled to tandem mass spectrometry). Five perfluorinatedcarboxylic acids (C6, C8–C11) and perfluorooctane sulfonate (PFOS) were selected as model analytes. In order to achieve the best extraction efficiency, some important factors including the amount of Fe{sub 3}O{sub 4}@mSiO{sub 2}-F{sub 17} microspheres added, adsorption time, type of elution solvent, eluting solvent volume and elution time were investigated. The ranges of the LOD were 0.02–0.05 ng mL{sup −1} for the six PFCs. The recovery of the optimized method varies from 83.13% to 92.42% for human serum samples.

  7. New Vanadium Compounds in Venezuela Heavy Crude Oil Detected by Positive-ion Electrospray Ionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry

    Science.gov (United States)

    Zhao, Xu; Shi, Quan; Gray, Murray R.; Xu, Chunming

    2014-06-01

    Metalloporphyrins are ubiquitous in nature, particularly iron porphyrins (hemes) and magnesium dihydroporphyrins or chlorophylls. Oxovanadium (IV) complexes of alkyl porphyrins are widely distributed in petroleum, oil shales and maturing sedimentary bitumen. Here we identify new vanadium compounds in Venezuela Orinoco heavy crude oil detected by Fourier transform-ion cyclotron resonance mass spectrometry (FT-ICR MS). These compounds likely have the main structure of porphyrin, with the addition of more aromatic rings, thiophene and amino functional groups, corresponding to molecular series of CnH2n-40N4V1O1 (36 <= n <= 58),CnH2n-42N4V1O1 (37 <= n <= 57),CnH2n-44N4V1O1 (38 <= n <= 59),CnH2n-46N4V1O1 (43 <= n <= 54),CnH2n-48N4V1O1 (45 <= n <= 55),CnH2n-38N4V1S1O1 (36 <= n <= 41),CnH2n-40N4V1S1O1 (35 <= n <= 51),CnH2n-42N4V1S1O1 (36 <= n <= 54),CnH2n-44N4V1S1O1 (41 <= n <= 55),CnH2n-46N4V1S1O1 (39 <= n <= 55),CnH2n-27N5V1O1 (29 <= n <= 40),CnH2n-29N5V1O1 (34 <= n <= 42),CnH2n-33N5V1O1 (31 <= n <= 38),CnH2n-35N5V1O1 (32 <= n <= 41),CnH2n-27N5V1O2 (32 <= n <= 41) and CnH2n-29N5V1O2 (33 <= n <= 42). These findings are significant for the understanding of the existing form of vanadium species in nature, and are helpful for enhancing the amount of information on palaeoenvironments and improving the level of applied basic theory for the processing technologies of heavy oils.

  8. Capture of Planetesimals into a Circumterrestrial Swarm

    Science.gov (United States)

    Weidenschilling, S. J.

    1985-01-01

    The lunar origin model considered in this report involves processing of protolunar material through a circumterrestrial swarm of particles. Once such a swarm has formed, it can gain mass by capturing infalling planetesimals and ejecta from giant impacts on the Earth, although the angular momentum supply from these sources remains a problem. The first stage of formation of a geocentric swarm by capture of planetesimals from initially heliocentric orbits is examined. The only plausible capture mechanism that is not dependent on very low approach velocities is the mutual collision of planetesimals passing within Earth's sphere of influence. The dissipation of energy in inelastic collisions or accretion events changes the value of the Jacobi parameter, allowing capture into bound geocentric orbits. This capture scenario was tested directly by many body numerical integration of planetesimal orbits in near Earth space.

  9. Overriding auditory attentional capture.

    Science.gov (United States)

    Dalton, Polly; Lavie, Nilli

    2007-02-01

    Attentional capture by color singletons during shape search can be eliminated when the target is not a feature singleton (Bacon & Egeth, 1994). This suggests that a "singleton detection" search strategy must be adopted for attentional capture to occur. Here we find similar effects on auditory attentional capture. Irrelevant high-intensity singletons interfered with an auditory search task when the target itself was also a feature singleton. However, singleton interference was eliminated when the target was not a singleton (i.e., when nontargets were made heterogeneous, or when more than one target sound was presented). These results suggest that auditory attentional capture depends on the observer's attentional set, as does visual attentional capture. The suggestion that hearing might act as an early warning system that would always be tuned to unexpected unique stimuli must therefore be modified to accommodate these strategy-dependent capture effects. PMID:17557587

  10. Neutron Capture Nucleosynthesis

    OpenAIRE

    Kiss, Miklos

    2016-01-01

    Heavy elements (beyond iron) are formed in neutron capture nucleosynthesis processes. We have proposed a simple unified model to investigate the neutron capture nucleosynthesis in arbitrary neutron density environment. We have also investigated what neutron density is required to reproduce the measured abundance of nuclei assuming equilibrium processes. We found both of these that the medium neutron density has a particularly important role at neutron capture nucleosynthesis. About these resu...

  11. Overriding auditory attentional capture

    OpenAIRE

    Dalton, Polly; Lavie, Nilli

    2007-01-01

    Attentional capture by color singletons during shape search can be eliminated when the target is not a feature singleton (Bacon & Egeth, 1994). This suggests that a "singleton detection" search strategy must be adopted for attentional capture to occur. Here we find similar effects on auditory attentional capture. Irrelevant high-intensity singletons interfered with an auditory search task when the target itself was also a feature singleton. However, singleton interference was eliminated when ...

  12. Application of neutron capture autoradiography to Boron Delivery seeking techniques for selective accumulation of boron compounds to tumor with intra-arterial administration of boron entrapped water-in-oil-in-water emulsion

    International Nuclear Information System (INIS)

    It is necessary to accumulate the 10B atoms selectively to the tumor cells for effective Boron Neutron Capture Therapy (BNCT). In order to achieve an accurate measurement of 10B accumulations in the biological samples, we employed a technique of neutron capture autoradiography (NCAR) of sliced samples of tumor tissues using CR-39 plastic track detectors. The CR-39 track detectors attached with the biological samples were exposed to thermal neutrons in the thermal column of the JRR3 of Japan Atomic Energy Agency (JAEA). We obtained quantitative NCAR images of the samples for VX-2 tumor in rabbit liver after injection of 10BSH entrapped water-in-oil-in-water (WOW) emulsion by intra-arterial injection via proper hepatic artery. The 10B accumulations and distributions in VX-2 tumor and normal liver of rabbit were investigated by means of alpha-track density measurements. In this study, we showed the selective accumulation of 10B atoms in the VX-2 tumor by intra-arterial injection of 10B entrapped WOW emulsion until 3 days after injection by using digitized NCAR images (i.e. alpha-track mapping).

  13. Optimized cleanup method for the determination of short chain polychlorinated n-alkanes in sediments by high resolution gas chromatography/electron capture negative ion-low resolution mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Gao Yuan; Zhang Haijun [Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China); Chen Jiping, E-mail: chenjp@dicp.ac.cn [Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China); Zhang Qing; Tian Yuzeng; Qi Peipei; Yu Zhengkun [Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China)

    2011-10-10

    Graphical abstract: The sediment sample could be purified by the optimized cleanup method, and satisfying cleanup efficiency was obtained. Highlights: {yields} The elution characters of sPCAs and interfering substances were evaluated on three adsorbents. {yields} An optimized cleanup method was developed for sPCAs with satisfying cleanup efficiency. {yields} The cleanup method combined with HRGC/ECNI-LRMS was applied for sPCAs analysis. {yields} The sPCAs levels range from 53.6 ng g{sup -1} to 289.3 ng g{sup -1} in tested sediment samples. - Abstract: The performances of three adsorbents, i.e. silica gel, neutral and basic alumina, in the separation of short chain polychlorinated n-alkanes (sPCAs) from potential interfering substances such as polychlorinated biphenyls (PCBs) and organochlorine pesticides were evaluated. To increase the cleanup efficiency, a two-step cleanup method using silica gel column and subsequent basic alumina column was developed. All the PCB and organochlorine pesticides could be removed by this cleanup method. The very satisfying cleanup efficiency of sPCAs has been achieved and the recovery in the cleanup method reached 92.7%. The method detection limit (MDL) for sPCAs in sediments was determined to be 14 ng g{sup -1}. Relative standard deviation (R.S.D.) of 5.3% was obtained for the mass fraction of sPCAs by analyzing four replicates of a spiked sediment sample. High resolution gas chromatography/electron capture negative ion-low resolution mass spectrometry (HRGC/ECNI-LRMS) was used for sPCAs quantification by monitoring [M-HCl]{center_dot}{sup -} ions. When applied to the sediment samples from the mouth of the Daliao River, the optimized cleanup method in conjunction with HRGC/ECNI-LRMS allowed for highly selective identifications for sPCAs. The sPCAs levels in sediment samples are reported to range from 53.6 ng g{sup -1} to 289.3 ng g{sup -1}. C{sub 10}- and C{sub 11}-PCAs are the dominant residue in most of investigated sediment

  14. Optimized cleanup method for the determination of short chain polychlorinated n-alkanes in sediments by high resolution gas chromatography/electron capture negative ion-low resolution mass spectrometry

    International Nuclear Information System (INIS)

    Graphical abstract: The sediment sample could be purified by the optimized cleanup method, and satisfying cleanup efficiency was obtained. Highlights: → The elution characters of sPCAs and interfering substances were evaluated on three adsorbents. → An optimized cleanup method was developed for sPCAs with satisfying cleanup efficiency. → The cleanup method combined with HRGC/ECNI-LRMS was applied for sPCAs analysis. → The sPCAs levels range from 53.6 ng g-1 to 289.3 ng g-1 in tested sediment samples. - Abstract: The performances of three adsorbents, i.e. silica gel, neutral and basic alumina, in the separation of short chain polychlorinated n-alkanes (sPCAs) from potential interfering substances such as polychlorinated biphenyls (PCBs) and organochlorine pesticides were evaluated. To increase the cleanup efficiency, a two-step cleanup method using silica gel column and subsequent basic alumina column was developed. All the PCB and organochlorine pesticides could be removed by this cleanup method. The very satisfying cleanup efficiency of sPCAs has been achieved and the recovery in the cleanup method reached 92.7%. The method detection limit (MDL) for sPCAs in sediments was determined to be 14 ng g-1. Relative standard deviation (R.S.D.) of 5.3% was obtained for the mass fraction of sPCAs by analyzing four replicates of a spiked sediment sample. High resolution gas chromatography/electron capture negative ion-low resolution mass spectrometry (HRGC/ECNI-LRMS) was used for sPCAs quantification by monitoring [M-HCl]·- ions. When applied to the sediment samples from the mouth of the Daliao River, the optimized cleanup method in conjunction with HRGC/ECNI-LRMS allowed for highly selective identifications for sPCAs. The sPCAs levels in sediment samples are reported to range from 53.6 ng g-1 to 289.3 ng g-1. C10- and C11-PCAs are the dominant residue in most of investigated sediment samples.

  15. Neutron Capture Nucleosynthesis

    CERN Document Server

    Kiss, Miklos

    2016-01-01

    Heavy elements (beyond iron) are formed in neutron capture nucleosynthesis processes. We have proposed a simple unified model to investigate the neutron capture nucleosynthesis in arbitrary neutron density environment. We have also investigated what neutron density is required to reproduce the measured abundance of nuclei assuming equilibrium processes. We found both of these that the medium neutron density has a particularly important role at neutron capture nucleosynthesis. About these results most of the nuclei can formed at medium neutron capture density environment e.g. in some kind of AGB stars. Besides these observations our model is capable to use educational purpose.

  16. Gadolinium atom on neutron capture therapy

    International Nuclear Information System (INIS)

    This report describes our measurements of gadolinium concentrations in several brain tumors obtained from fresh surgical specimens, as compared with corresponding concentrations in the blood. Moreover we tried to find out if the gadolinium concentration is high enough to use this compound in the treatment of brain tumors by neutron capture therapy. (J.P.N.)

  17. Speciation of four selenium compounds using high performance liquid chromatography with on-line detection by inductively coupled plasma mass spectrometry or flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Pedersen, G.A. [National Food Agency of Denmark, Institute of Food Chemistry and Nutrition, Moerkhoej Bygade 19, DK-2860 Soeborg (Denmark); Larsen, E.H. [National Food Agency of Denmark, Institute of Food Chemistry and Nutrition, Moerkhoej Bygade 19, DK-2860 Soeborg (Denmark)

    1997-07-01

    An analytical method for the speciation of selenomethionine, selenocystine, selenite and selenate by high performance liquid chromatography (HPLC) with atomic spectrometric detection is presented. An organic polymeric strong anion exchange column was used as the stationary phase in combination with an aqueous solution of 6 mmol L{sup -1} of salicylate ion at pH 8.5 as the mobile phase which allowed the isocratic separation of the four selenium analytes within 8 minutes. The separated selenium species were detected on-line by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma mass spectrometry (ICP-MS). The signal-to-noise ratio of the FAAS detector was optimized using a hydrogen-argon entrained-air flame and a slotted-tube atom trap (STAT) in the flame. The limit of detection (3 {sigma}) achieved by the HPLC-FAAS system was 1 mg L{sup -1} of selenium (100 {mu}L injections) for each of the four selenium species. More powerful selenium detection was achieved using an ELAN 5000 ICP-MS instrument. Selenium was measured at m/z = 82. The ICP-MS signal intensity was enhanced by a factor of 3-4 after addition of 3% methanol to the chromatographic mobile phase and by using an increased plasma power input of 1300 W. The limit of detection achieved under these conditions was 1 {mu}g L{sup -1} (100 {mu}L injections). The HPLC-ICP-MS system was used for selenium speciation of selenite and selenate in aqueous solutions during a BCR certification exercise and for selenium speciation in the certified reference material, BCR No. 402 White Clover. Extraction experiments revealed that the selenium species in the biological material were extractable only in the presence of water in the extraction medium. The results indicated that selenate and a compound of unknown identity U were present in the plant sample. (orig.). With 5 figs., 5 tabs.

  18. Determination of butyl-, phenyl-, octyl- and tributylmonomethyltin compounds in a marine environment (Bay of Bengal, India) using gas chromatography-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Rajendran, R B; Tao, H; Miyazaki, A; Ramesh, R; Ramachandran, S

    2001-12-01

    Organotin compounds (butyl-, phenyl-, octyl- and tributylmonomethyltin) and inorganic tin were quantified in sea-water and sediments from two harbours and several locations on the southeast coast of India using highly sensitive and selective gas chromatography-inductively coupled plasma mass spectrometry (GC-ICP-MS), adopting new extraction and analytical techniques with extremely low detection limits (water, 0.019-0.85 pg l(-1); sediment, 0.23-0.48 ng g(-1)). The concentrations of monobutyltin (MBT), dibutyltin (DBT) and tributyltin (TBT) in sea-water from Tuticorin harbour varied from 0.64 to 4.97, 3.0 to 26.8 and 0.3 to 30.4 ng Sn l(-1), respectively. MBT, DBT and TBT in sediments from harbour areas ranged from 1.6 to 393, 1.3 to 394 and ND (not detected) to 1280 ng Sn g(-1) (dry weight), respectively. Natural methylation in both harbours was established by quantifying tributylmonomethyltin (TBMMT) residues (sea-water, ND-0.19 ng Sn l(-1); sediment, ND-765 ng Sn g(-1) dry weight). In sea-water, octyltins were also determined as monooctyltin (MOT) > dioctyltin (DOT) > trioctyltin (TOT). Butyltin contamination in commercial harbours is evident, but other coastal waters are not contaminated with organotin residues. The high concentration of inorganic tin in estuarine sediment indicates an elevated rate of debutylation in the estuarine environment. Both methylation and debutylation of TBT in Chennai harbour were greater than in Tuticorin harbour. A significant correlation (r2 = 0.75) between total butyltin and organic carbon contents in sediment was found. To our knowledge, this is the first report on the distribution of butyltins and methylated butyltin in sea-water and sediment and octyltins in sea-water in the Indian marine environment. PMID:11785637

  19. Use of microextraction by packed sorbents and gas chromatography-mass spectrometry for the determination of polyamines and related compounds in urine.

    Science.gov (United States)

    Casas Ferreira, Ana María; Moreno Cordero, Bernardo; Crisolino Pozas, Ángel Pedro; Pérez Pavón, José Luis

    2016-04-29

    A novel methodology for the determination of ornithine, putrescine, cadaverine, spermidine and gamma-amino butyric acid in urine samples has been developed. The method uses in situ aqueous derivatization followed by automated microextraction by packed sorbent coupled to a gas chromatography-mass spectrometry system equipped with a programmed temperature vaporizer. This instrumental configuration minimizes sample manipulation due to from the mixing of the reagents, the process is completely automated. The analytes were derivatized using ethyl chloroformate as derivatization reagent. The reaction occurred in aqueous medium and was carried out in 1min in the vial of an autosampler used to perform microextraction by packed sorbent. The parameters affecting derivatization, extraction and separation were optimized in order to obtain maximum sensitivity. Calibration curves were obtained for five calibration levels in three different matrices. All the calibration models displayed good linearity, with R(2) values higher than 0.95. The validity of the models was checked using ANOVA, and it was observed that they did not exhibit any lack of fit. Repeatability and reproducibility was evaluated, with values below 15% in both cases. LOD and LOQ values were found to be in the low μg/L level. Influence of the matrix was confirmed, thus quantification was performed using the standard additions method and normalization to IS. The method developed was applied to the analysis of these compounds in urine samples from healthy individuals and cancer diagnosed patients (Internal Medicine Unit of the Virgen de la Vega Hospital, Salamanca, Spain). Significant differences (Mann-Whitney U test) were observed for putrescine and ornithine concentrations. PMID:27036212

  20. Quantitative analysis of phenolic compounds in Chinese hawthorn (Crataegus spp.) fruits by high performance liquid chromatography-electrospray ionisation mass spectrometry.

    Science.gov (United States)

    Liu, Pengzhan; Kallio, Heikki; Lü, Deguo; Zhou, Chuansheng; Yang, Baoru

    2011-08-01

    Eleven major phenolic compounds (hyperoside, isoquercitrin, chlorogenic acid, ideain, epicatechin, two procyanidin (PA) dimers, three PA trimers and a PA dimer-hexoside) were quantified in the fruits of 22 cultivars/origins of three species of the Chinese hawthorn (Crataegus spp.) by HPLC-ESI-MS-SIR. Hyperoside (0.1-0.8mg/g dry mass [DM]), isoquercitrin (0.1-0.3mg/g DM), chlorogenic acid (0.2-1.6mg/g DM), epicatechin (0.9-11.7mg/g DM), PA B2 (0.7-12.4mg/g DM), PA dimer II (0.1-1.5mg/g DM), PA trimer I (0.1-2.7mg/g DM), PA trimer II (0.7-6.9mg/g DM), PA trimer III (0.01-1.2mg/g DM) and a PA dimer-hexoside (trace-1.1mg/g DM) were detected in all the samples. Ideain (0.0-0.7mg/g DM) was found in all the samples except Crataegus scabrifolia. Significant correlations between the contents of individual PA aglycons were observed (r>0.9, P<0.01). A strong correlation between flavonols was also shown (r=0.71, P<0.01). Fruits of Crataegus pinnatifida var. major had higher contents of PAs but lower contents of flavonols compared with Crataegus brettschneideri. The fruits of C. scabrifolia contained the highest level of PA dimer-hexoside, which was present in trace amounts in the fruits of C. pinnatifida. PMID:25214140

  1. Analysis and quantitation of volatile organic compounds emitted from plastics used in museum construction by evolved gas analysis-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Samide, Michael J; Smith, Gregory D

    2015-12-24

    Construction materials used in museums for the display, storage, and transportation of artwork must be assessed for their tendency to emit harmful pollution that could potentially damage cultural treasures. Traditionally, a subjective metals corrosion test known as the Oddy test has been widely utilized in museums for this purpose. To augment the Oddy test, an instrumental sampling approach based on evolved gas analysis (EGA) coupled to gas chromatography (GC) with mass spectral (MS) detection has been implemented for the first time to qualitatively identify off-gassed pollutants under specific conditions. This approach is compared to other instrumental methods reported in the literature. This novel application of the EGA sampling technique yields several benefits over traditional testing, including rapidity, high sensitivity, and broad detectability of volatile organic compounds (VOCs). Furthermore, unlike other reported instrumental approaches, the EGA method was used to determine quantitatively the amount of VOCs emitted by acetate resins and polyurethane foams under specific conditions using both an external calibration method as well as surrogate response factors. EGA was successfully employed to rapidly characterize emissions from 12 types of common plastics. This analysis is advocated as a rapid pre-screening method to rule out poorly performing materials prior to investing time and energy in Oddy testing. The approach is also useful for rapid, routine testing of construction materials previously vetted by traditional testing, but which may experience detrimental formulation changes over time. As an example, a case study on batch re-orders of rigid expanded poly(vinyl chloride) board stock is presented. PMID:26687162

  2. Reversible Ionic Liquids as Double-Action Solvents for Efficient CO{sub 2} Capture

    Energy Technology Data Exchange (ETDEWEB)

    Charles Eckert; Charles Liotta

    2011-09-30

    We have developed a novel class of CO{sub 2} capture solvents, Reversible Ionic Liquids (RevILs), that offer high absorption capacity through two modes of capture: chemical reaction (chemisorption) and physical solubility (physisorption). These solvents are silicon containing alkaline compounds such as silylamines that form a liquid salt (ionic liquid) upon reaction with CO{sub 2}. Subsequently, modest elevations in temperature reverse the reaction and yield pure CO{sub 2} for sequestration. By incorporating Si in the molecules we have reduced the viscosity, thereby improving the mass transfer rates of CO{sub 2} absorption/desorption and decreasing the processing costs for pumping the solvent. In this project, we have made systematic changes to the structure of these compounds to improve several physical and thermodynamic properties important for CO{sub 2} capture. Through these structure-property paradigms, we have obtained a RevIL which requires only a third of the energy required by conventional aqueous MEA process for 90% CO{sub 2} capture.

  3. Reversible Ionic Liquids as Double-Action Solvents for Efficient CO2 Capture

    Energy Technology Data Exchange (ETDEWEB)

    Eckert, Charles; Liotta, Charles

    2011-09-30

    We have developed a novel class of CO{sub 2} capture solvents, Reversible Ionic Liquids (RevILs), that offer high absorption capacity through two modes of capture: chemical reaction (chemisorption) and physical solubility (physisorption). These solvents are silicon containing alkaline compounds such as silylamines that form a liquid salt (ionic liquid) upon reaction with CO{sub 2}. Subsequently, modest elevations in temperature reverse the reaction and yield pure CO{sub 2} for sequestration. By incorporating Si in the molecules we have reduced the viscosity, thereby improving the mass transfer rates of CO{sub 2} absorption/desorption and decreasing the processing costs for pumping the solvent. In this project, we have made systematic changes to the structure of these compounds to improve several physical and thermodynamic properties important for CO{sub 2} capture. Through these structure-property paradigms, we have obtained a RevIL which requires only a third of the energy required by conventional aqueous MEA process for 90% CO{sub 2} capture.

  4. CAPTURE OF TROJANS BY JUMPING JUPITER

    International Nuclear Information System (INIS)

    Jupiter Trojans are thought to be survivors of a much larger population of planetesimals that existed in the planetary region when planets formed. They can provide important constraints on the mass and properties of the planetesimal disk, and its dispersal during planet migration. Here, we tested a possibility that the Trojans were captured during the early dynamical instability among the outer planets (aka the Nice model), when the semimajor axis of Jupiter was changing as a result of scattering encounters with an ice giant. The capture occurs in this model when Jupiter's orbit and its Lagrange points become radially displaced in a scattering event and fall into a region populated by planetesimals (that previously evolved from their natal transplanetary disk to ∼5 AU during the instability). Our numerical simulations of the new capture model, hereafter jump capture, satisfactorily reproduce the orbital distribution of the Trojans and their total mass. The jump capture is potentially capable of explaining the observed asymmetry in the number of leading and trailing Trojans. We find that the capture probability is (6-8) × 10–7 for each particle in the original transplanetary disk, implying that the disk contained (3-4) × 107 planetesimals with absolute magnitude H disk ∼ 14-28 MEarth, is consistent with the mass deduced from recent dynamical simulations of the planetary instability.

  5. Neutrino Masses

    CERN Document Server

    Weinheimer, Christian

    2013-01-01

    The various experiments on neutrino oscillation evidenced that neutrinos have indeed non-zero masses but cannot tell us the absolute neutrino mass scale. This scale of neutrino masses is very important for understanding the evolution and the structure formation of the universe as well as for nuclear and particle physics beyond the present Standard Model. Complementary to deducing constraints on the sum of all neutrino masses from cosmological observations two different methods to determine the neutrino mass scale in the laboratory are pursued: the search for neutrinoless double $\\beta$-decay and the direct neutrino mass search by investigating single $\\beta$-decays or electron captures. The former method is not only sensitive to neutrino masses but also probes the Majorana character of neutrinos and thus lepton number violation with high sensitivity. Currently quite a few experiments with different techniques are being constructed, commissioned or are even running, which aim for a sensitivity on the neutrino ...

  6. Search for resonant double-electron capture

    Energy Technology Data Exchange (ETDEWEB)

    Eliseev, Sergey; Blaum, Klaus; Roux, Christian [Max-Planck-Institut fuer Kernphysik, Heidelberg (Germany); Block, Michael; Minaya Ramirez, Enrique [GSI Helmholtzzentrum fuer Schwerionenforschung GmbH, Darmstadt (Germany); Droese, Christian; Schweikhard, Lutz [Institut fuer Physik, Ernst-Moritz-Arndt-Universitaet, Greifswald (Germany); Nesterenko, Dmitriy; Novikov, Yuri [PNPI, St. Petersburg (Russian Federation); Zuber, Kai [Institut fuer Kern- und Teilchenphysik, Technische Universitaet, Dresden (Germany)

    2013-07-01

    It is still unknown whether neutrinos are Dirac or Majorana particles. An answer to this question can be obtained from neutrinoless double-electron capture. An observation of this process would prove that the neutrino is a Majorana particle. A measurement of the half-life of this process would allow a determination of the effective Majorana neutrino mass. In the search for the nuclide with the largest probability for neutrinoless double-electron capture, we have determined the Q-values of several potentially suitable nuclides with SHIPTRAP by Penning-trap mass-ratio measurements. The ECEC-transition in {sup 152}Gd has been determined to have the smallest half-life of 10{sup 26} years for a 1 eV neutrino mass among all known 0νECEC-transitions, which makes {sup 152}Gd the most promising candidate for the search for neutrino-less double electron capture. This contribution summarizes the recent experimental results.

  7. Fusion–fission dynamics studies using mass distribution as a probe

    Indian Academy of Sciences (India)

    T K Ghosh; A Chaudhuri; K Banerjee; S Bhattacharya; C Bhattacharya; S Kundu; G Mukherjee; R Pandey; T K Rana; P Roy; T Roy; V Srivastava; P Bhattacharya

    2015-08-01

    Study of quasifission reaction mechanism and shell effects in compound nuclei has important implications on the synthesis of superheavy elements (SHE). Using the major accelerator facilities available in India, quasifission reaction mechanism and shell effects in compound nuclei were studied extensively. Fission fragment mass distribution was used as a probe. Two factors, viz., nuclear orientation and direction of mass flow of the initial dinuclear system after capture were seen to determine the extent of quasifission. From the measurement of fragment mass distribution in -induced reaction on actinide targets, it was possible to constrain the excitation energy at which nuclear shell effect washed out.

  8. Identification of organic sulfur compounds in coal bitumen obtained by different extraction techniques using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Machado, Maria Elisabete; Cappelli Fontanive, Fernando; Bastos Caramao, Elina; Alcaraz Zini, Claudia [Universidade Federal do Rio Grande do Sul, Instituto de Quimica, Porto Alegre, RS (Brazil); Oliveira, Jose Vladimir de [URI, Universidade Regional Integrada do Alto Uruguai e das Missoes, Erechim, RS (Brazil)

    2011-11-15

    The determination of organic sulfur compounds (OSC) in coal is of great interest. Technically and operationally these compounds are not easily removed and promote corrosion of equipment. Environmentally, the burning of sulfur compounds leads to the emission of SO{sub x} gases, which are major contributors to acid rain. Health-wise, it is well known that these compounds have mutagenic and carcinogenic properties. Bitumen can be extracted from coal by different techniques, and use of gas chromatography coupled to mass spectrometric detection enables identification of compounds present in coal extracts. The OSC from three different bitumens were tentatively identified by use of three different extraction techniques: accelerated solvent extraction (ASE), ultrasonic extraction (UE), and supercritical-fluid extraction (SFE). Results obtained from one-dimensional gas chromatography (1D GC) coupled to quadrupole mass spectrometric detection (GC-qMS) and from two-dimensional gas chromatography with time-of-flight mass spectrometric detection (GC x GC-TOFMS) were compared. By use of 2D GC, a greater number of OSC were found in ASE bitumen than in SFE and UE bitumens. No OSC were identified with 1D GC-qMS, although some benzothiophenes and dibenzothiophenes were detected by use of EIM and SIM modes. GC x GC-TOFMS applied to investigation of OSC in bitumens resulted in analytical improvement, as more OSC classes and compounds were identified (thiols, sulfides, thiophenes, naphthothiophenes, benzothiophenes, and benzonaphthothiophenes). The roof-tile effect was observed for OSC and PAH in all bitumens. Several co-elutions among analytes and with matrix interferents were solved by use of GC x GC. (orig.)

  9. Carbon Capture and Storage

    NARCIS (Netherlands)

    Benson, S.M.; Bennaceur, K.; Cook, P.; Davison, J.; Coninck, H. de; Farhat, K.; Ramirez, C.A.; Simbeck, D.; Surles, T.; Verma, P.; Wright, I.

    2012-01-01

    Emissions of carbon dioxide, the most important long-lived anthropogenic greenhouse gas, can be reduced by Carbon Capture and Storage (CCS). CCS involves the integration of four elements: CO 2 capture, compression of the CO2 from a gas to a liquid or a denser gas, transportation of pressurized CO 2

  10. CAPTURED India Country Evaluation

    NARCIS (Netherlands)

    O'Donoghue, R.; Brouwers, J.H.A.M.

    2012-01-01

    This report provides the findings of the India Country Evaluation and is produced as part of the overall CAPTURED End Evaluation. After five years of support by the CAPTURED project the End Evaluation has assessed that results are commendable. I-AIM was able to design an approach in which health fol

  11. Quantitative analysis of nitrogen containing compounds in microalgae based bio-oils using comprehensive two-dimensional gas-chromatography coupled to nitrogen chemiluminescence detector and time of flight mass spectrometer.

    Science.gov (United States)

    Toraman, Hilal E; Franz, Kristina; Ronsse, Frederik; Van Geem, Kevin M; Marin, Guy B

    2016-08-19

    Insight in the composition of the algae derived bio-oils is crucial for the development of efficient conversion processes and better upgrading strategies for microalgae. Comprehensive two-dimensional gas chromatography (GC×GC) coupled to nitrogen chemiluminescence detector (NCD) and time-of-flight mass spectrometer (TOF-MS) allows to obtain the detailed quantitative composition of the nitrogen containing compounds in the aqueous and the organic fraction of fast pyrolysis bio-oils from microalgae. Normal phase (apolar×mid-polar) and reverse phase column (polar×apolar) combination are investigated to optimize the separation of the detected nitrogen containing compounds. The reverse phase column combination gives the most detailed information in terms of the nitrogen containing compounds. The combined information from the GC×GC-TOF-MS (qualitative) and GC×GC-NCD (quantitative) with the use of a well-chosen internal standard, i.e. caprolactam, enables the identification and quantification of nitrogen containing compounds belonging to 13 different classes: amines, imidazoles, amides, imides, nitriles, pyrazines, pyridines, indoles, pyrazoles, pyrimidines, quinolines, pyrimidinediones and other nitrogen containing compounds which were not assigned to a specific class. The aqueous fraction mostly consists of amines (4.0wt%) and imidazoles (2.8wt%) corresponding to approximately 80wt% of the total identified nitrogen containing compounds. On the other hand, the organic fraction shows a more diverse distribution of nitrogen containing compounds with the majority of the compounds quantified as amides (3.0wt%), indoles (2.0wt%), amines (1.7wt%) and imides (1.3wt%) corresponding to approximately 65wt% of the total identified nitrogen containing compounds. PMID:27432785

  12. The Mass Attenuation Coefficients, Electronic, Atomic, and Molecular Cross Sections, Effective Atomic Numbers, and Electron Densities for Compounds of Some Biomedically Important Elements at 59.5 keV

    OpenAIRE

    Burcu Akça; Erzeneoğlu, Salih Z.

    2014-01-01

    The mass attenuation coefficients for compounds of biomedically important some elements (Na, Mg, Al, Ca, and Fe) have been measured by using an extremely narrow collimated-beam transmission method in the energy 59.5 keV. Total electronic, atomic, and molecular cross sections, effective atomic numbers, and electron densities have been obtained by using these results. Gamma-rays of 241Am passed through compounds have been detected by a high-resolution Si(Li) detector and by using energy dispers...

  13. Muon capture in hydrogen

    International Nuclear Information System (INIS)

    In this lecture I will mainly speak about the recent results obtained by the Saclay-CERN-Bologna (SCB) collaboration on the muon capture rate at rest in liquid hydrogen.In the first talk I shall first briefly remind the theoretical description of the capture process, then describe the experimental difficulties and procedures and finally present the results obtained. In the second talk I shall compare them to other capture experiments on the proton and present the informations that are provided by muon capture in hydrogen, especially for the PCAC hypothesis, the second class currents and the μ-e universality. Finally I shall present the possible muon capture experiments on the proton that could still be undertaken in order to improve our present knowledge of the subject

  14. Simultaneous determination of phenolic compounds and saponins in quinoa (Chenopodium quinoa Willd) by a liquid chromatography-diode array detection-electrospray ionization-time-of-flight mass spectrometry methodology.

    Science.gov (United States)

    Gómez-Caravaca, Ana María; Segura-Carretero, Antonio; Fernández-Gutiérrez, Alberto; Caboni, Maria Fiorenza

    2011-10-26

    A new liquid chromatography methodology coupled to a diode array detector and a time-of-flight mass spectrometer has been developed for the simultaneous determination of phenolic compounds and saponins in quinoa (Chenopodium quinoa Willd). This method has allowed the simultaneous determination of these two families of compounds with the same analytical method for the first time. A fused-core column C18 has been used, and the analysis has been performed in less than 27 min. Both chromatographic and electrospray ionization time-of-flight mass spectrometry parameters have been optimized to improve the sensitivity and to maximize the number of compounds detected. A validation of the method has also been carried out, and free and bound polar fractions of quinoa have been studied. Twenty-five compounds have been tentatively identified and quantified in the free polar fraction, while five compounds have been tentatively identified and quantified in the bound polar fraction. It is important to highlight that 1-O-galloyl-β-D-glucoside, acacetin, protocatechuic acid 4-O-glucoside, penstebioside, ethyl-m-digallate, (epi)-gallocatechin, and canthoside have been tentatively identified for the first time in quinoa. Free phenolic compounds have been found to be in the range of 2.746-3.803 g/kg of quinoa, while bound phenolic compounds were present in a concentration that varies from 0.139 and 0.164 g/kg. Indeed, saponins have been found to be in a concentration that ranged from 5.6 to 7.5% of the total composition of whole quinoa flour. PMID:21905641

  15. Organics Captured from Comet Wild 2 by the Stardust Spacecraft

    Energy Technology Data Exchange (ETDEWEB)

    Stanford, S A; Aleon, J; O' D. Alexander, C M; Araki, T; Bajt, S; Baratta, G A; Borg, J; Brucato, J R; Burchell, M J; Busemann, H; Butterworth, A; Clemett, S J; Cody, G; Colangeli, L; Cooper, G; D' Hendecourt, L; Djouadi, Z; Dworkin, J P; Ferrini, G; Fleckenstein, H; Flynn, G; Franchi, I A; Fries, M; Gilles, M K; Glavin, D P; Gounelle, M; Grossemy, F; Jacobsen, C; Keller, L P; Kilcoyne, A D; Leitner, J; Matrajt, G; Meibom, A; Mennella, V; Mostefaoui, S; Nittler, L R; Palumbo, M E; Robert, F; Rotundi, A; Snead, C J; Spencer, M K; Steele, A; Stephan, T; Tyliszczak, T; Westphal, A J; Wirick, S; Wopenka, B; Yabuta, H; Zare, R N; Zolensky, M

    2006-10-11

    Organics found in Comet Wild 2 samples show a heterogeneous and unequilibrated distribution in abundance and composition. Some organics are similar, but not identical, to those in interplanetary dust particles (IDPs) and carbonaceous meteorites. A class of aromatic-poor organic material is also present. The organics are rich in O and N compared to meteoritic organics. Aromatic compounds are present, but the samples tend to be relatively poorer in aromatics than meteorites and IDPs. D and {sup 15}N suggest that some organics have an interstellar/protostellar heritage. While the variable extent of modification of these materials by impact capture is not yet fully constrained, a remarkably diverse suite of organic compounds is present and identifiable within the returned samples. Comets are small bodies that accreted in the outer Solar System during its formation (1) and thus may consist of preserved samples of the ''starting materials'' from which the Solar System was made. Organic materials are expected to be present in cometary samples (2) and may include molecules made and/or modified in stellar outflows, the interstellar medium, and the protosolar nebula, as well as by parent body processing within the comet. The presence of organic compounds in comets and their ejecta is of astrobiological interest since their delivery to the early Earth may have played an important role in the origin of life on Earth (3). An overview of the Stardust Mission and the collection and recovery of Wild 2 samples is provided elsewhere (4,5). We describe the results obtained from the returned samples by the Stardust Organics Preliminary Examination Team (PET). Samples were studied using a wide range of analytical techniques, including two-step laser desorption laser ionization mass spectrometry (L{sub 2}MS), Liquid Chromatography with UV Fluorescence Detection and Time of Flight Mass Spectrometry (LC-FD/TOF-MS), Scanning Transmission X-ray Microscopy (STXM), X

  16. Mass spectrometric immunoassay

    Science.gov (United States)

    Nelson, Randall W; Williams, Peter; Krone, Jennifer Reeve

    2007-12-04

    Rapid mass spectrometric immunoassay methods for detecting and/or quantifying antibody and antigen analytes utilizing affinity capture to isolate the analytes and internal reference species (for quantification) followed by mass spectrometric analysis of the isolated analyte/internal reference species. Quantification is obtained by normalizing and calibrating obtained mass spectrum against the mass spectrum obtained for an antibody/antigen of known concentration.

  17. Characterization of sulfur and nitrogen compounds in Brazilian petroleum derivatives using ionic liquid capillary columns in comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometric detection.

    Science.gov (United States)

    Cappelli Fontanive, Fernando; Souza-Silva, Érica Aparecida; Macedo da Silva, Juliana; Bastos Caramão, Elina; Alcaraz Zini, Claudia

    2016-08-26

    Diesel and naphtha samples were analyzed using ionic liquid (IL) columns to evaluate the best column set for the investigation of organic sulfur compounds (OSC) and nitrogen(N)-containing compounds analyses with comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry detector (GC×GC/TOFMS). Employing a series of stationary phase sets, namely DB-5MS/DB-17, DB-17/DB-5MS, DB-5MS/IL-59, and IL-59/DB-5MS, the following parameters were systematically evaluated: number of tentatively identified OSC, 2D chromatographic space occupation, number of polyaromatic hydrocarbons (PAH) and OSC co-elutions, and percentage of asymmetric peaks. DB-5MS/IL-59 was chosen for OSC analysis, while IL59/DB-5MS was chosen for nitrogen compounds, as each stationary phase set provided the best chromatographic efficiency for these two classes of compounds, respectively. Most compounds were tentatively identified by Lee and Van den Dool and Kratz retention indexes, and spectra-matching to library. Whenever available, compounds were also positively identified via injection of authentic standards. PMID:27488721

  18. Isolation of phenolic compounds from hop extracts using polyvinylpolypyrrolidone: characterization by high-performance liquid chromatography-diode array detection-electrospray tandem mass spectrometry.

    Science.gov (United States)

    Magalhães, Paulo J; Vieira, Joana S; Gonçalves, Luís M; Pacheco, João G; Guido, Luís F; Barros, Aquiles A

    2010-05-01

    The aim of the present work was the development of a suitable methodology for the separation and determination of phenolic compounds in the hop plant. The developed methodology was based on the sample purification by adsorption of phenolic compounds from the matrix to polyvinylpolypyrrolidone (PVPP) and subsequent desorption of the adsorbed polyphenols with acetone/water (70:30, v/v). At last, the extract was analyzed by HPLC-DAD and HPLC-ESI-MS/MS. The first phase of this work consisted of the study of the adsorption behavior of several classes of phenolic compounds (e.g. phenolic acids, flavonols, and flavanols) by PVPP in model solutions. It has been observed that the process of adsorption of the different phenolic compounds to PVPP (at low concentrations) is differentiated, depending on the structure of the compound (number of OH groups, aromatic rings, and stereochemistry hindrance). For example, within the phenolic acids class (benzoic, p-hydroxybenzoic, protocatechuic and gallic acids) the PVPP adsorption increases with the number of OH groups of the phenolic compound. On the other hand, the derivatization of OH groups (methylation and glycosylation) resulted in a greatly diminished binding. The use of PVPP revealed to be very efficient for adsorption of several phenolic compounds such as catechin, epicatechin, xanthohumol and quercetin, since high adsorption and recovery values were obtained. The methodology was further applied for the extraction and isolation of phenolic compounds from hops. With this methodology, it was possible to obtain high adsorption values (>or=80%) and recovery yield values (>or=70%) for the most important phenolic compounds from hops such as xanthohumol, catechin, epicatechin, quercetin and kaempferol glycosides, and in addition it allows the identification of about 30 phenolic compounds by HPLC-DAD and HPLC-ESI-MS/MS. PMID:19913228

  19. Speciation of butyltin compounds in environmental and biological samples using headspace single drop microextraction coupled with gas chromatography-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Xiao, Qin; Hu, Bin; He, Man

    2008-11-21

    A method based on headspace single drop microextraction (HS-SDME) in combination with gas chromatography-inductively coupled plasma mass spectrometry (GC-ICP-MS) was proposed for the speciation analysis of butyltin compounds in environmental and biological samples. The sodium tetraethylborate (NaBEt4) and sodium tetrahydroborate (NaBH4) were used as the derivatizing reagent for in situ derivatization of the butyltins. For the two derivatizations, the HS-SDME parameters such as organic solvent, drop volume, sample pH, stirring rate, temperature, extraction time and the ionic strength were examined systematically. The analytical performance including the linearity ranges, limits of detection (LODs) and reproducibilities of the two derivatizations were compared under the respective optimized conditions. Derivatization with NaBEt(4) proved to be more sensitive and robust than that with NaBH4, leading to the LODs of 1.4 ng/L for MBT, 1.8 ng/L for DBT and 0.8 ng/L for TBT. The reproducibilities, expressed as relative standard deviations (RSDs), were in the range of 1.1-5.3% (c=1 microg/L, n=3). With tripropyltin (TPrT) as internal standard, HS-SDME-GC-ICP-MS with NaBEt(4) derivatization was applied for the speciation analysis of butyltins in real seawater and shellfish samples. The butyltins found in the real-world samples are 31ng/L MBT, 79 ng/L DBT and 32 ng/L TBT for seawater, and 11.6-30.4 ng/g MBT, 11.8-8.9 ng/g DBT and 12.8-52.6 ng/g TBT for different shellfish samples. For validation, the developed method was also employed for the speciation analysis of butyltins in certified reference material (CRM) of PACS-2 sediment, and the determined values are in a good agreement with the certified values. The developed method is simple, rapid, sensitive, and cost-effective and provides an attractive alternative for butyltins speciation in biological and environmental samples with complex matrix. PMID:18922539

  20. Improved quantification of livestock associated odorous volatile organic compounds in a standard flow-through system using solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Yang, Xiuyan; Zhu, Wenda; Koziel, Jacek A; Cai, Lingshuang; Jenks, William S; Laor, Yael; Leeuwen, J Hans van; Hoff, Steven J

    2015-10-01

    Aerial emissions of odorous volatile organic compounds (VOCs) are an important nuisance factor from livestock production systems. Reliable air sampling and analysis methods are needed to develop and test odor mitigation technologies. Quantification of VOCs responsible for livestock odor remains an analytical challenge due to physicochemical properties of VOCs and the requirement for low detection thresholds. A new air sampling and analysis method was developed for testing of odor/VOCs mitigation in simulated livestock emissions system. A flow-through standard gas generating system simulating odorous VOCs in livestock barn emissions was built on laboratory scale and tested to continuously generate ten odorous VOCs commonly defining livestock odor. Standard VOCs included sulfur VOCs (S-VOCs), volatile fatty acids (VFAs), and p-cresol. Solid-phase microextraction (SPME) was optimized for sampling of diluted odorous gas mixtures in the moving air followed by gas chromatography-mass spectrometry (GC-MS) analysis. CAR/PDMS 85μm fiber was shown to have the best sensitivity for the target odorous VOCs. A practical 5-min sampling time was selected to ensure optimal extraction of VFAs and p-cresol, as well as minimum displacement of S-VOCs. Method detection limits ranged from 0.39 to 2.64ppbv for S-VOCs, 0.23 to 0.77ppbv for VFAs, and 0.31ppbv for p-cresol. The method developed was applied to quantify VOCs and odorous VOC mitigation with UV light treatment. The measured concentrations ranged from 20.1 to 815ppbv for S-VOCs, 10.3 to 315ppbv for VFAs, and 4.73 to 417ppbv for p-cresol. Relative standard deviations between replicates ranged from 0.67% to 12.9%, 0.50% to 11.4%, 0.83% to 5.14% for S-VOCs, VFAs, and p-cresol, respectively. This research shows that a simple manual SPME sampler could be used successfully for quantification of important classes of odorous VOCs at concentrations relevant for real aerial emissions from livestock operations. PMID:26456221

  1. Environment assisted electron capture

    International Nuclear Information System (INIS)

    Electrons scattering off isolated atoms or positive atomic ions may be captured in the non-resonant photorecombination or resonant dielectronic recombination processes with the excess energy carried off by a photon. We demonstrate that in a medium a new interatomic process becomes important, where in the electron capture by an atom or atomic ion the energy is transferred to a neigbouring species ionising it. We discuss different manifestations of this interatomic Coulombic electron capture and estimate its efficiency for a number of realistic systems.

  2. High resolution mass spectrometry imaging reveals the occurrence of phenylphenalenone-type compounds in red paracytic stomata and red epidermis tissue of Musa acuminata ssp. zebrina cv. 'Rowe Red'.

    Science.gov (United States)

    Hölscher, Dirk; Fuchser, Jens; Knop, Katrin; Menezes, Riya C; Buerkert, Andreas; Svatoš, Aleš; Schubert, Ulrich S; Schneider, Bernd

    2015-08-01

    The banana epidermis and in particular their stomata are conducive sites for the penetration of pathogenic fungi which can severely limit global banana production. The red pseudostem of the ornamental banana Musa acuminata ssp. zebrina cv. 'Rowe Red' was used to study the chemical constituents of the epidermal cell layer using matrix-free laser desorption/ionization Fourier transform ion cyclotron resonance mass spectrometric imaging (LDI-FT-ICR-MSI). The high resolution of this technique allowed phenylphenalenone-type compounds to be located in single plant cells. Some of these secondary metabolites were identified as constitutive compounds and found in specialized epidermal cells in banana pseudostem tissue. Especially the red paracytic stomata revealed higher signal intensities of certain phenylphenalenones than normal epidermis cells. The ease of detection of polycyclic aromatic compounds on the cellular level is discussed with regard to future investigations of plant-pathogen interactions. PMID:26004822

  3. A quantitative structure- property relationship of gas chromatographic/mass spectrometric retention data of 85 volatile organic compounds as air pollutant materials by multivariate methods

    Directory of Open Access Journals (Sweden)

    Sarkhosh Maryam

    2012-05-01

    Full Text Available Abstract A quantitative structure-property relationship (QSPR study is suggested for the prediction of retention times of volatile organic compounds. Various kinds of molecular descriptors were calculated to represent the molecular structure of compounds. Modeling of retention times of these compounds as a function of the theoretically derived descriptors was established by multiple linear regression (MLR and artificial neural network (ANN. The stepwise regression was used for the selection of the variables which gives the best-fitted models. After variable selection ANN, MLR methods were used with leave-one-out cross validation for building the regression models. The prediction results are in very good agreement with the experimental values. MLR as the linear regression method shows good ability in the prediction of the retention times of the prediction set. This provided a new and effective method for predicting the chromatography retention index for the volatile organic compounds.

  4. Conjugates of polyhedral boron compounds with carbohydrates. Communication 3. The first synthesis of a conjugate of the dodecaborate anion with a disaccharide lactose as a potential agent for boron neutron capture therapy of cancer

    International Nuclear Information System (INIS)

    An approach is reported which affords conjugates of the dodecaborate anion with practically any oligosaccharide derivative containing amino group. The conjugate was synthesized by condensation of N-glycyl-β-lactosyl amine with dodecaborate carboxy derivative, [B12H11O(CH2)4CO2]3-·3Bu4N+, in (2:1) methanol-water mixture in the presence of DMT-MM as a condensing agent. The product was obtained in 57% yield and characterized by 1H, 13C, 11B{1H} NMR and mass-spectra

  5. Capture of planetesimals into a circumterrestrial swarm

    Energy Technology Data Exchange (ETDEWEB)

    Weidenschilling, S.J.

    1984-01-01

    The lunar origin model considered involves processing of protolunar material through a circumterrestrial swarm of particles. Once such a swarm has formed, it can gain mass by capturing infalling planetesimals and ejecta from giant impacts on the Earth, although the angular momentum supply from these sources remains a problem. Examined is the first stage of formation of a geocentric swarm by capture of planetesimals from initialy heliocentric orbits. The only plausible capture mechanism that is not dependent on very low approach velocities is the mutual collision of planetesimals passing within Earth's sphere of influence. This capture scenario was tested directly by many body numerical integration of planetesimal orbits in near Earth space. Results agree that the systematic contribution of angular momentum is insufficient to maintain an orbiting swarm under heavy bombardment. Thus, a circumterrestrial swarm can be formed rather easily, but is hard to sustain because the mean net angular momentum of a many body swarm is small.

  6. Activists versus Captured Regulators

    OpenAIRE

    Daubanes, Julien; Rochet, Jean-Charles

    2013-01-01

    We analyze the consequences of activism in a regulated industry where the regulator has been captured by the industry. Unlike ordinary economic agents, activists are insensitive to monetary incentives. Moreover, they are less well informed than regulators and their actions generate dead-weight costs. Yet we find that activism may increase social welfare because it disciplines captured regulators and reduces the social cost of imperfect regulatory systems.

  7. Muon capture by tritium

    International Nuclear Information System (INIS)

    The muon capture rate is computed with realistic wave function for the initial tritium nuclei (Faddeev equations on configuration space with realistic potentials), and plane wave approximation for the final three neutrons, with the effective Hamiltonian of Fujii and Primakoff for muon capture and via a non energy weighted sum rule. Such a forbidden transition is hoped to be a probe for exchange current contributions

  8. Characterisation of Phenolic Compounds in South African Plum Fruits (Prunus salicina Lindl.) using HPLC Coupled with Diode-Array, Fluorescence, Mass Spectrometry and On-Line Antioxidant Detection

    OpenAIRE

    Dalene de Beer; Elizabeth Joubert; Alet Venter

    2013-01-01

    Phenolic compounds are abundant secondary metabolites in plums, with potential health benefits believed to be due to their antioxidant activity, amongst others. Phenolic characterisation of South African Prunus salicina Lindl. plums is necessary to fully evaluate their potential health benefits. An HPLC method using diode-array detection (DAD) for quantification of phenolic compounds was improved and fluorescence detection (FLD) was added for quantification of flavan-3-ols. Validation of the ...

  9. Analytical and statistical approaches to preselect relevant organic compounds in the non-target screening by coupling passive sampling and high resolution mass spectrometry: application to groundwater

    OpenAIRE

    Coralie, Soulier; Catherine, Berho; Anne, Togola

    2015-01-01

    International audience One of ongoing challenge is to protect and preserve water resources. This involves an increased monitoring and the characterization of micropollutants, emerging substances and their metabolites or transformation products. Emerging compounds are mostly released by wastewaters discharge into surface waters and then into other environmental compartment. All these compounds are present in complex mixture at low concentration, implying the need of specific analytical meth...

  10. Emissions of organic compounds from technosphere articles : Measurements and modeling of mass transfer from consumer goods and building materials to air and water

    OpenAIRE

    Holmgren, Tomas

    2013-01-01

    This thesis describes the development of a generic model for predicting the emissions of organic compounds from materials used in the manufacture of various goods and products. Many products contain organic substances that are not bound to the matrix formed by their constituent materials and are thus able to dissociate from the material and become transferred into the surrounding environment. A wide range of materials and products are used in modern societies, and many compounds deriving from...

  11. Identification and quantification of gaseous organic compounds emitted from biomass burning using two-dimensional gas chromatography/time-of-flight mass spectrometry

    OpenAIRE

    Hatch, L. E.; Luo, W.; Pankow, J. F.; Yokelson, R. J.; C. E. Stockwell; K. C. Barsanti

    2014-01-01

    The current understanding of secondary organic aerosol (SOA) formation within biomass burning (BB) plumes is limited by the incomplete identification and quantification of the non-methane organic compounds (NMOCs) emitted from such fires. Gaseous organic compounds were collected on sorbent cartridges during laboratory burns as part of the fourth Fire Lab at Missoula Experiment (FLAME-4), with analysis by two-dimensional gas chromatography/time-of-flight mas...

  12. Review of fission produce capture measurements at the Oak Ridge Electron Laser Accelerator (ORELA)

    International Nuclear Information System (INIS)

    The 40-meter capture system of R.L. Macklin at ORELA has been used to measure capture cross sections for over eighty isotopes between A = 75 and 161, the primary mass region of interest for fission products. This review outlines the primary features of the capture system, lists the isotopes measured and their references, and describes recent changes incorporated in the capture system

  13. Neutron capture therapy for melanoma

    International Nuclear Information System (INIS)

    The development of boron-containing compounds which localize selectively in tumor may require a tumor-by-tumor type of approach that exploits any metabolic pathways unique to the particular type of tumor. Melanin-producing melanomas actively transport and metabolize aromatic amino acids for use as precursors in the synthesis of the pigment melanin. It has been shown that the boron-containing amino acid analog p-borono-phenylalanine (BPA) is selectively accumulated in melanoma tissue, producing boron concentrations in tumor that are within the range estimated to be necessary for successful boron neutron capture therapy (BNCT). We report here the results of therapy experiments carried out at the Brookhaven Medical Research Reactor (BMRR). 21 refs., 5 figs., 3 tabs

  14. Workshop on neutron capture therapy

    Energy Technology Data Exchange (ETDEWEB)

    Fairchild, R.G.; Bond, V.P. (eds.)

    1986-01-01

    Potentially optimal conditions for Neutron Capture Therapy (NCT) may soon be in hand due to the anticipated development of band-pass filtered beams relatively free of fast neutron contaminations, and of broadly applicable biomolecules for boron transport such as porphyrins and monoclonal antibodies. Consequently, a number of groups in the US are now devoting their efforts to exploring NCT for clinical application. The purpose of this Workshop was to bring these groups together to exchange views on significant problems of mutual interest, and to assure a unified and effective approach to the solutions. Several areas of preclinical investigation were deemed to be necessary before it would be possible to initiate clinical studies. As neither the monomer nor the dimer of sulfhydryl boron hydride is unequivocally preferable at this time, studies on both compounds should be continued until one is proven superior.

  15. Workshop on neutron capture therapy

    International Nuclear Information System (INIS)

    Potentially optimal conditions for Neutron Capture Therapy (NCT) may soon be in hand due to the anticipated development of band-pass filtered beams relatively free of fast neutron contaminations, and of broadly applicable biomolecules for boron transport such as porphyrins and monoclonal antibodies. Consequently, a number of groups in the US are now devoting their efforts to exploring NCT for clinical application. The purpose of this Workshop was to bring these groups together to exchange views on significant problems of mutual interest, and to assure a unified and effective approach to the solutions. Several areas of preclinical investigation were deemed to be necessary before it would be possible to initiate clinical studies. As neither the monomer nor the dimer of sulfhydryl boron hydride is unequivocally preferable at this time, studies on both compounds should be continued until one is proven superior

  16. Methods of Analysis by the U.S. Geological Survey Organic Geochemistry Research Group-Update and Additions to the Determination of Chloroacetanilide Herbicide Degradation Compounds in Water Using High-Performance Liquid Chromatography/Mass Spectrometry

    Science.gov (United States)

    Lee, E.A.; Kish, J.L.; Zimmerman, L.R.; Thurman, E.

    2001-01-01

    An analytical method using high-performance liquid chromatography/mass spectrometry (HPLC/MS) was developed by the U.S. Geological Survey in 1999 for the analysis of selected chloroacetanilide herbicide degradation compounds in water. These compounds were acetochlor ethane sulfonic acid (ESA), acetochlor oxanilic acid (OXA), alachlor ESA, alachlor OXA, metolachlor ESA, and metolachlor OXA. The HPLC/MS method was updated in 2000, and the method detection limits were modified accordingly. Four other degradation compounds also were added to the list of compounds that can be analyzed using HPLC/MS; these compounds were dimethenamid ESA, dimethenamid OXA, flufenacet ESA, and flufenacet OXA. Except for flufenacet OXA, good precision and accuracy were demonstrated for the updated HPLC/MS method in buffered reagent water, surface water, and ground water. The mean HPLC/MS recoveries of the degradation compounds from water samples spiked at 0.20 and 1.0 ?g/L (microgram per liter) ranged from 75 to 114 percent, with relative standard deviations of 15.8 percent or less for all compounds except flufenacet OXA, which had relative standard deviations ranging from 11.3 to 48.9 percent. Method detection levels (MDL's) using the updated HPLC/MS method varied from 0.009 to 0.045 ?g/L, with the flufenacet OXA MDL at 0.072 ?g/L. The updated HPLC/MS method is valuable for acquiring information about the fate and transport of the parent chloroacetanilide herbicides in water.

  17. A strategy for identification and structural characterization of compounds from Gardenia jasminoides by integrating macroporous resin column chromatography and liquid chromatography-tandem mass spectrometry combined with ion-mobility spectrometry.

    Science.gov (United States)

    Wang, Lu; Liu, Shu; Zhang, Xueju; Xing, Junpeng; Liu, Zhiqiang; Song, Fengrui

    2016-06-24

    In this paper, an analysis strategy integrating macroporous resin (AB-8) column chromatography and high performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS/MS) combined with ion mobility spectrometry (IMS) was proposed and applied for identification and structural characterization of compounds from the fruits of Gardenia jasminoides. The extracts of G. jasminoides were separated by AB-8 resin column chromatography combined with reversed phase liquid chromatography (C18 column) and detected by electrospray ionization tandem mass spectrometry. Additionally, ion mobility spectrometry (IMS) was employed as a supplementary separation technique to discover previously undetected isomers from the fruits of G. jasminoides. A total of 71 compounds, including iridoids, flavonoids, triterpenes, monoterpenoids, carotenoids and phenolic acids were identified by the characteristic high resolution mass spectrometry and the ESI-MS/MS fragmentations. In conclusion, the IMS-MS technique achieved the separation of isomers in crocin-3 and crocin-4 according to their acquired mobility drift times differing from classical analysis by mass spectrometry. The proposed strategy can be used as a highly sensitive and efficient procedure for identification and separation isomeric components in extracts of herbal medicines. PMID:27208986

  18. Mass spectrometry.

    Science.gov (United States)

    Burlingame, A. L.; Johanson, G. A.

    1972-01-01

    Review of the current state of mass spectrometry, indicating its unique importance for advanced scientific research. Mass spectrometry applications in computer techniques, gas chromatography, ion cyclotron resonance, molecular fragmentation and ionization, and isotope labeling are covered. Details are given on mass spectrometry applications in bio-organic chemistry and biomedical research. As the subjects of these applications are indicated alkaloids, carbohydrates, lipids, terpenes, quinones, nucleic acid components, peptides, antibiotics, and human and animal metabolisms. Particular attention is given to the mass spectra of organo-inorganic compounds, inorganic mass spectrometry, surface phenomena such as secondary ion and electron emission, and elemental and isotope analysis. Further topics include mass spectrometry in organic geochemistry, applications in geochronology and cosmochemistry, and organic mass spectrometry.

  19. Migration of odorous compounds from adhesives used in market samples of food packaging materials by chromatography olfactometry and mass spectrometry (GC-O-MS).

    Science.gov (United States)

    Vera, Paula; Canellas, Elena; Nerín, Cristina

    2014-02-15

    Adhesives are commonly used in the manufacture of multilayer food packaging materials. Although they are not in direct contact with the packed food, their compounds may migrate from the adhesive through the substrates to the food. The aim of this work is to determine the migrant concentration in order to evaluate the possible human risk and also to determine if this migration could affect the organoleptic properties of packed food. For this purpose, a total of 12 market samples of multilayer materials (laminates) for packaging dry food (tomatoes, cakes, cookies, breadcrumbs, flour or salt) or fresh food (pizza and pastry) produced with 5 different adhesives were analysed by GC-O-MS. A total of 25 different compounds from adhesives were detected in these laminates. Seventy-six percentage of these compounds migrated into a dry food simulant (Tenax®). Furthermore, compounds with concentrations below the MS detection limit were detected by sniffers with a high modified frequency (MF%). Acetic acid, butyric acid and cyclohexanol with vinegar, cheese and camphor odours were the most abundant compounds. All migration data were below the specific migration limits (SML) and threshold toxicological concern (TTC) recommended values according to the Cramer classification. PMID:24128473

  20. ALLocator: an interactive web platform for the analysis of metabolomic LC-ESI-MS datasets, enabling semi-automated, user-revised compound annotation and mass isotopomer ratio analysis.

    Directory of Open Access Journals (Sweden)

    Nikolas Kessler

    Full Text Available Adduct formation, fragmentation events and matrix effects impose special challenges to the identification and quantitation of metabolites in LC-ESI-MS datasets. An important step in compound identification is the deconvolution of mass signals. During this processing step, peaks representing adducts, fragments, and isotopologues of the same analyte are allocated to a distinct group, in order to separate peaks from coeluting compounds. From these peak groups, neutral masses and pseudo spectra are derived and used for metabolite identification via mass decomposition and database matching. Quantitation of metabolites is hampered by matrix effects and nonlinear responses in LC-ESI-MS measurements. A common approach to correct for these effects is the addition of a U-13C-labeled internal standard and the calculation of mass isotopomer ratios for each metabolite. Here we present a new web-platform for the analysis of LC-ESI-MS experiments. ALLocator covers the workflow from raw data processing to metabolite identification and mass isotopomer ratio analysis. The integrated processing pipeline for spectra deconvolution "ALLocatorSD" generates pseudo spectra and automatically identifies peaks emerging from the U-13C-labeled internal standard. Information from the latter improves mass decomposition and annotation of neutral losses. ALLocator provides an interactive and dynamic interface to explore and enhance the results in depth. Pseudo spectra of identified metabolites can be stored in user- and method-specific reference lists that can be applied on succeeding datasets. The potential of the software is exemplified in an experiment, in which abundance fold-changes of metabolites of the l-arginine biosynthesis in C. glutamicum type strain ATCC 13032 and l-arginine producing strain ATCC 21831 are compared. Furthermore, the capability for detection and annotation of uncommon large neutral losses is shown by the identification of (γ-glutamyl dipeptides in

  1. Quantification of the Triazole Antifungal Compounds Voriconazole and Posaconazole in Human Serum or Plasma Using Liquid Chromatography Electrospray Tandem Mass Spectrometry (HPLC-ESI-MS/MS).

    Science.gov (United States)

    Molinelli, Alejandro R; Rose, Charles H

    2016-01-01

    Voriconazole and posaconazole are triazole antifungal compounds used in the treatment of fungal infections. Therapeutic drug monitoring of both compounds is recommended in order to guide drug dosing to achieve optimal blood concentrations. In this chapter we describe an HPLC-ESI-MS/MS method for the quantification of both compounds in human plasma or serum following a simple specimen preparation procedure. Specimen preparation consists of protein precipitation using methanol and acetonitrile followed by a cleanup step that involves filtration through a cellulose acetate membrane. The specimen is then injected into an HPLC-ESI-MS/MS equipped with a C18 column and separated over an acetonitrile gradient. Quantification of the drugs in the specimen is achieved by comparing the response of the unknown specimen to that of the calibrators in the standard curve using multiple reaction monitoring. PMID:26660172

  2. Muon capture at PSI

    CERN Document Server

    Winter, Peter

    2010-01-01

    Measuring the rate of muon capture in hydrogen provides one of the most direct ways to study the axial current of the nucleon. The MuCap experiment uses a negative muon beam stopped in a time projection chamber operated with ultra-pure hydrogen gas. Surrounded by a decay electron detector, the lifetime of muons in hydrogen can be measured to determine the singlet capture rate Lambda_s to a final precision of 1%. The capture rate determines the nucleon's pseudoscalar form factor g_p. A first result, g_p = 7.3 +- 1.1, has been published and the final analysis of the full statistics will reduce the error by a factor of up to 3. Muon capture on the deuteron probes the weak axial current in the two-nucleon system. Within the framework of effective field theories the calculation of such two-nucleon processes involving the axial current requires the knowledge of one additional low energy constant which can be extracted from the doublet capture rate Lambda_d. The same constant then allows to model-independently calcu...

  3. Recent advances in neutron capture therapy (NCT)

    Energy Technology Data Exchange (ETDEWEB)

    Fairchild, R.G.

    1985-01-01

    The application of the /sup 10/B(n,..cap alpha..)/sup 7/Li reaction to cancer radiotherapy (Neutron Capture therapy, or NCT) has intrigued investigators since the discovery of the neutron. This paper briefly summarizes data describing recently developed boronated compounds with evident tumor specificity and extended biological half-lives. The implication of these compounds to NCT is evaluated in terms of Therapeutic Gain (TG). The optimization of NCT using band-pass filtered beams is described, again in terms of TG, and irradiation times with these less intense beams are estimated. 24 refs., 3 figs., 3 tabs.

  4. Neutron capture therapy at Brookhaven National Laboratory

    International Nuclear Information System (INIS)

    Application of the 10B(n,α)7Li reaction to cancer radiotherapy (Neutron Capture therapy, or NCT) has intrigued investigators since shortly after the discovery of the neutron. This paper summarizes data describing recently developed boronated compounds designed to serve as vehicles for boron transport to tumor. Whole-body (mouse) Neutron Capture Radiograms (NCR) of some of the most promising compounds are presented; these graphically demonstrate selective uptake in tumor, at times varying from hours to days post administration. Comparison is made to the ubiquitous distribution of inorganic boron compounds used in the first clinical trials of NCT. Since some compounds are now available that allow physiological targeting of boron to tumor at concentrations adequate for therapy, the NCR technique can be used to evaluate important questions concerning the microdistribution of boron within the tumor. The implication of these compounds to NCT is evaluated in terms of Therapeutic Gain (TG). The optimization of NCT by using band-pass filtered neutron beams is described, again in terms of TG, and irradiation times with these less intense beams are estimated. 35 references, 12 figures, 4 tables

  5. Muon Capture in Deuterium

    CERN Document Server

    Ricci, P; Mosconi, B; Smejkal, J

    2009-01-01

    Model dependence of the capture rates of the negative muon capture in deuterium is studied starting from potential models and the weak two-body meson exchange currents constructed in the tree approximation and also from an effective field theory. The tree one-boson exchange currents are derived from the hard pion chiral Lagrangians of the $N \\Delta \\pi \\rho \\omega a_1$ system. If constructed in conjunction with the one-boson exchange potentials, the capture rates can be calculated consistently. On the other hand, the effective field theory currents, constructed within the heavy baryon chiral perturbation theory, contain a low energy constant $\\hat d ^R$ that cannot be extracted from data at the one-particle level nor determined from the first principles. Comparative analysis of the results for the doublet transition rate allows us to extract the constant $\\hat d ^R$.

  6. US Spacesuit Knowledge Capture

    Science.gov (United States)

    Chullen, Cinda; Thomas, Ken; McMann, Joe; Dolan, Kristi; Bitterly, Rose; Lewis, Cathleen

    2011-01-01

    The ability to learn from both the mistakes and successes of the past is vital to assuring success in the future. Due to the close physical interaction between spacesuit systems and human beings as users, spacesuit technology and usage lends itself rather uniquely to the benefits realized from the skillful organization of historical information; its dissemination; the collection and identification of artifacts; and the education of those in the field. The National Aeronautics and Space Administration (NASA), other organizations and individuals have been performing United States (U.S.) Spacesuit Knowledge Capture since the beginning of space exploration. Avenues used to capture the knowledge have included publication of reports; conference presentations; specialized seminars; and classes usually given by veterans in the field. More recently the effort has been more concentrated and formalized whereby a new avenue of spacesuit knowledge capture has been added to the archives in which videotaping occurs engaging both current and retired specialists in the field presenting technical scope specifically for education and preservation of knowledge. With video archiving, all these avenues of learning can now be brought to life with the real experts presenting their wealth of knowledge on screen for future learners to enjoy. Scope and topics of U.S. spacesuit knowledge capture have included lessons learned in spacesuit technology, experience from the Gemini, Apollo, Skylab and Shuttle programs, hardware certification, design, development and other program components, spacesuit evolution and experience, failure analysis and resolution, and aspects of program management. Concurrently, U.S. spacesuit knowledge capture activities have progressed to a level where NASA, the National Air and Space Museum (NASM), Hamilton Sundstrand (HS) and the spacesuit community are now working together to provide a comprehensive closed-looped spacesuit knowledge capture system which includes

  7. Information, Media and Elections: Incentives for Media Capture

    OpenAIRE

    Serena Marianna Drufuca

    2014-01-01

    Media play an essential role in democracy by making available valuable information for electoral decisions. In a framework of political economy of mass media, I inquiry the possibility of capture by rent-seeking o cers in a heterogeneous electoral environment. This allow me to discuss when relevant information is traded, when government captures media and what e ect this has on political outcomes. I nd media capture to be a pervasive phenomenon which implies minimum costs on politicians' side...

  8. Neutron capture cross sections from Surrogate measurements

    OpenAIRE

    Scielzo N.D.; Dietrich F.S.; Escher J.E.

    2010-01-01

    The prospects for determining cross sections for compound-nuclear neutron-capture reactions from Surrogate measurements are investigated. Calculations as well as experimental results are presented that test the Weisskopf-Ewing approximation, which is employed in most analyses of Surrogate data. It is concluded that, in general, one has to go beyond this approximation in order to obtain (n,γ) cross sections of sufficient accuracy for most astrophysical and nuclear-energy applications.

  9. Neutron capture cross sections from Surrogate measurements

    Directory of Open Access Journals (Sweden)

    Scielzo N.D.

    2010-03-01

    Full Text Available The prospects for determining cross sections for compound-nuclear neutron-capture reactions from Surrogate measurements are investigated. Calculations as well as experimental results are presented that test the Weisskopf-Ewing approximation, which is employed in most analyses of Surrogate data. It is concluded that, in general, one has to go beyond this approximation in order to obtain (n,γ cross sections of sufficient accuracy for most astrophysical and nuclear-energy applications.

  10. An exploratory comparative study of volatile compounds in exhaled breath and emitted by skin using selected ion flow tube mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Turner, C.; Parekh, B.; Walton, Ch.; Španěl, Patrik; Smith, D.; Evans, M.

    2008-01-01

    Roč. 22, č. 4 (2008), s. 526-532. ISSN 0951-4198 Institutional research plan: CEZ:AV0Z40400503 Keywords : SIFT-MS * volatile compounds * aldehydes Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.772, year: 2008

  11. Rapid method for the simultaneous detection of boar taint compounds by means of solid phase microextraction coupled to gas chromatography/mass spectrometry.

    Science.gov (United States)

    Verplanken, Kaat; Wauters, Jella; Van Durme, Jim; Claus, Dirk; Vercammen, Joeri; De Saeger, Sarah; Vanhaecke, Lynn

    2016-09-01

    Because of animal welfare issues, the voluntary ban on surgical castration of male piglets, starting January 2018 was announced in a European Treaty. One viable alternative is the fattening of entire male pigs. However, this can cause negative consumer reactions due to the occurrence of boar taint and possibly lead to severe economic losses in pig husbandry. In this study, headspace solid phase microextraction (HS-SPME) coupled to GC-MS was used in the development and optimization of a candidate method for fast and accurate detection of the boar taint compounds. Remarkably fast extraction (45s) of the boar taint compounds from adipose tissue was achieved by singeing the fat with a soldering iron while released volatiles were extracted in-situ using HS-SPME. The obtained method showed good performance characteristics after validation according to CD 2002/657/EC and ISO/IEC 17025 guidelines. Moreover, cross-validation with an in-house UHPLC-HR-Orbitrap-MS method showed good agreement between an in-laboratory method and the new candidate method for the fast extraction and detection of skatole and androstenone, which emphasizes the accuracy of this new SPME-GC-MS method. Threshold detection of the boar taint compounds on a portable GC-MS could not be achieved. However, despite the lack of sensitivity obtained on the latter instrument, a very fast method with run-to-run time of 3.5min for the detection of the boar taint compounds was developed. PMID:27492596

  12. Identification of Aroma-active Compounds in Essential Oil from Uncaria Hook by Gas Chromatography- Mass Spectrometry and Gas Chromatography-Olfactometry.

    Science.gov (United States)

    Iwasa, Megumi; Nakaya, Satoshi; Maki, Yusuke; Marumoto, Shinsuke; Usami, Atsushi; Miyazawa, Mitsuo

    2015-01-01

    The chemical composition of essential oil extracted from Uncaria Hook ("Chotoko" in Japanese), the branch with curved hook of the herbal medicine Uncaria rhynchophylla has been investigated by GC and GC-MS analyses. Eighty-four compounds, representing 90.8% of the total content was identified in oil obtained from Uncaria Hook. The main components i were (E)-cinnamaldehyde (13.4%), α-copaene (8.0%), methyl eugenol (6.8%), δ-cadinene (5.3%), and curcumene (3.6%). The important key aroma-active compounds in the oil were detected by gas chromatography-olfactometry (GC-O) and aroma extract dilution analysis (AEDA), using the flavor dilution (FD) factor to express the odor potency of each compounds. Furthermore, the odor activity value (OAV) has been used as a measure of the relative contribution of each compound to the aroma of the Uncaria Hook oil. The GC-O and AEDA results showed that α-copaene (FD = 4, OAV = 4376), (E)-linalool oxide (FD = 64, OAV = 9.1), and methyl eugenol (FD = 64, OAV = 29) contributed to the woody and spicy odor of Uncaria Hook oil, whereas furfural (FD = 8, OAV = 4808) contributed to its sweet odor. These results warrant further investigations of the application of essential oil from Uncaria Hook in the phytochemical and medicinal fields. PMID:26179003

  13. Sexual behavior and male volatile compounds in wild and mass-reared strains of the Mexican fruit fly Anastrepha ludens (Diptera: Tephritidae) held under different colony management regimes.

    Science.gov (United States)

    Bosa, Carlos Felipe; Cruz-López, Leopoldo; Zepeda-Cisneros, Cristina Silvia; Valle-Mora, Javier; Guillén-Navarro, Karina; Liedo, Pablo

    2016-02-01

    We compared the calling and mating behavior and volatile release of wild males Anastrepha ludens (Loew) with males from 4 mass-reared strains: (i) a standard mass-reared colony (control), (ii) a genetic sexing strain (Tap-7), (iii) a colony started from males selected on their survival and mating competitiveness abilities (selected), and (iv) a hybrid colony started by crossing wild males with control females. Selected and wild males were more competitive, achieving more matings under field cage conditions. Mass-reared strains showed higher percentages of pheromone calling males under field conditions except for Tap-7 males, which showed the highest percentages of pheromone calling males under laboratory cage conditions. For mature males of all strains, field-cage calling behavior increased during the last hour before sunset, with almost a 2 fold increase exhibited by wild males during the last half hour. The highest peak mating activity of the 4 mass-reared strains occurred 30 min earlier than for wild males. By means of solid phase microextraction (SPME) plus gas chromatography-mass spectrometry (GC-MS), the composition of volatiles released by males was analyzed and quantified. Wild males emitted significantly less amounts of (E,E)-α-farnesene but emitted significantly more amounts of (E,E)-suspensolide as they aged than mass-reared males. Within the 4 mass-reared strains, Tap-7 released significantly more amounts of (E,E)-α-farnesene and hybrid more of (E,E)-suspensolide. Differences in chemical composition could be explained by the intrinsic characteristics of the strains and the colony management regimes. Characterization of calling behavior and age changes of volatile composition between wild and mass-reared strains could explain the differences in mating competitiveness and may be useful for optimizing the sterile insect technique in A. ludens. PMID:25339372

  14. CAPTURED End Evaluation Synthesis Report

    NARCIS (Netherlands)

    Brouwers, J.H.A.M.

    2012-01-01

    This report provides the findings of the Synthesis Study of the CAPTURED Evaluation and is produced as part of the overall CAPTURED End Evaluation. After five years of support by the CAPTURED project the three CAPTURED partners have achieved commendable results. Ten lessons learned are formulated th

  15. Theory of electron capture

    International Nuclear Information System (INIS)

    The historical development of a theoretical model for the electron-capture detector, sometimes called the 'classical' model, is presented and the model as it stands today is described. This is followed by a comparison of the model with experimental data obtained with other techniques since the early development of the theory and finally a section on correlations and predictions is presented. (Auth.)

  16. The Mass Attenuation Coefficients, Electronic, Atomic, and Molecular Cross Sections, Effective Atomic Numbers, and Electron Densities for Compounds of Some Biomedically Important Elements at 59.5 keV

    Directory of Open Access Journals (Sweden)

    Burcu Akça

    2014-01-01

    Full Text Available The mass attenuation coefficients for compounds of biomedically important some elements (Na, Mg, Al, Ca, and Fe have been measured by using an extremely narrow collimated-beam transmission method in the energy 59.5 keV. Total electronic, atomic, and molecular cross sections, effective atomic numbers, and electron densities have been obtained by using these results. Gamma-rays of 241Am passed through compounds have been detected by a high-resolution Si(Li detector and by using energy dispersive X-ray fluorescence spectrometer (EDXRF. Obtained results have been compared with theoretically calculated values of WinXCom and FFAST. The relative difference between the experimental and theoretical values are −9.4% to +11.9% with WinXCom and −11.8% to +11.7% FFAST. Results have been presented and discussed in this paper.

  17. Silver-Mordenite for Radiologic Gas Capture from Complex Streams: Dual Catalytic CH3I Decomposition and I Confinement

    Energy Technology Data Exchange (ETDEWEB)

    Tina M. Nenoff; Mark Rodriguez; Nick Soelberg; Karena W. Chapman

    2014-12-01

    The effective capture and storage of radiological iodine (129I) remains a strong concern for safe nuclear waste storage and safe nuclear energy. Silver-containing mordenite (MOR) is a longstanding benchmark for iodine capture. In nuclear fuel reprocessing scenarios, complex gas streams will be present and the need for high selectivity of all iodine containing compounds is of the utmost importance for safety and the environment. In particular, a molecular level understanding of the sorption of organic iodine compounds is not well understood. Here we probe the structure and distribution of methyl iodide sorbed by silver-containing MOR using a combination of crystallographic and materials characterization techniques including: infrared spectroscopy, thermogravimetric analysis with mass spectrometry, Micro-X-ray Fluorescence, powder X-ray diffraction analysis, and pair distribution function analysis. The iodine is captured inside the MOR pore in the form of AgI nanoparticles, that is consistent with the pores sizes of the MOR, indicating that the molecule is both physically and chemically captured in the Ag-MOR. The organic component is surface catalyzed by the zeolite via the formation of Surface Methoxy Species (SMS) that result in downstream organics of dimethyl ether and methanol formation.

  18. Characterization of volatile organic compounds (VOCs) in Asian and north American pollution plumes during INTEX-B: identification of specific Chinese air mass tracers

    OpenAIRE

    B. Barletta; Meinardi, S.; Simpson, I J; Atlas, E. L.; A. J. Beyersdorf; A. K. Baker; N. J. Blake; Yang, M..; Midyett, J. R.; Novak, B. J.; McKeachie, R. J.; H. E. Fuelberg; Sachse, G. W.; M. A. Avery; Campos, T.

    2009-01-01

    We present results from the Intercontinental Chemical Transport Experiment – Phase B (INTEX-B) aircraft mission conducted in spring 2006. By analyzing the mixing ratios of volatile organic compounds (VOCs) measured during the second part of the field campaign, together with kinematic back trajectories, we were able to identify five plumes originating from China, four plumes from other Asian regions, and three plumes from the United States. To identify specific tracers for the different air ma...

  19. Headspace Solid-Phase Microextraction Gas Chromatography-Mass Spectrometry and Gas Chromatography-Olfactometry Analysis of Volatile Compounds in Pineapple Breads

    OpenAIRE

    Seye Lasekan; Kalla Reddi Mohan Naidu; Ola Lasekan; Saw Ying

    2012-01-01

    Sensorial analysis of pineapple breads (conventionally baked, Cpb; fully baked frozen, Fpb and partially baked, Ppb) showed no significant differences in terms of aroma and taste. On the contrary, the scores for the overall quality between the partially baked and conventionally baked breads showed significant (p < 0.05) differences. At the same time, headspace analysis using a solid-phase microextraction (SPME) method identified 59 volatile compounds. The results of the aroma extracts ...

  20. Automatic on-line monitoring of atmospheric volatile organic compounds: Gas chromatography-mass spectrometry and gas chromatography-flame ionization detection as complementary systems

    International Nuclear Information System (INIS)

    Traditionally air quality networks have been carrying out the continuous, on-line measurement of volatile organic compounds (VOC) in ambient air with GC-FID. In this paper some identification and coelution problems observed while using this technique in long-term measurement campaigns are described. In order to solve these problems a GC-MS was set up and operated simultaneously with a GC-FID for C2-C11 VOCs measurement. There are few on-line, unattended, long term measurements of atmospheric VOCs performed with GC-MS. In this work such a system has been optimized for that purpose, achieving good repeatability, linearity, and detection limits of the order of the GC-FID ones, even smaller in some cases. VOC quantification has been made by using response factors, which is not frequent in on-line GC-MS. That way, the identification and coelution problems detected in the GC-FID, which may led to reporting erroneous data, could be corrected. The combination of GC-FID and GC-MS as complementary techniques for the measurement of speciated VOCs in ambient air at sub-ppbv levels is proposed. Some results of the measurements are presented, including concentration values for some compounds not found until now on public ambient air VOC databases, which were identified and quantified combining both techniques. Results may also help to correct previously published VOC data with wrongly identified compounds by reprocessing raw chromatographic data.