WorldWideScience

Sample records for capture compound mass

  1. Capture compound mass spectrometry--a powerful tool to identify novel c-di-GMP effector proteins.

    Science.gov (United States)

    Laventie, Benoît-Joseph; Nesper, Jutta; Ahrné, Erik; Glatter, Timo; Schmidt, Alexander; Jenal, Urs

    2015-01-01

    Considerable progress has been made during the last decade towards the identification and characterization of enzymes involved in the synthesis (diguanylate cyclases) and degradation (phosphodiesterases) of the second messenger c-di-GMP. In contrast, little information is available regarding the molecular mechanisms and cellular components through which this signaling molecule regulates a diverse range of cellular processes. Most of the known effector proteins belong to the PilZ family or are degenerated diguanylate cyclases or phosphodiesterases that have given up on catalysis and have adopted effector function. Thus, to better define the cellular c-di-GMP network in a wide range of bacteria experimental methods are required to identify and validate novel effectors for which reliable in silico predictions fail. We have recently developed a novel Capture Compound Mass Spectrometry (CCMS) based technology as a powerful tool to biochemically identify and characterize c-di-GMP binding proteins. This technique has previously been reported to be applicable to a wide range of organisms(1). Here we give a detailed description of the protocol that we utilize to probe such signaling components. As an example, we use Pseudomonas aeruginosa, an opportunistic pathogen in which c-di-GMP plays a critical role in virulence and biofilm control. CCMS identified 74% (38/51) of the known or predicted components of the c-di-GMP network. This study explains the CCMS procedure in detail, and establishes it as a powerful and versatile tool to identify novel components involved in small molecule signaling.

  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. 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.

  4. 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

  5. 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...

  6. 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...

  7. Neutrino Mass, Electron Capture and the Shake-off Contributions

    CERN Document Server

    Faessler, Amand; Simkovic, Fedor

    2016-01-01

    Electron capture can determine the electron neutrino mass, while the beta decay of Tritium measures the electron antineutrino mass and the neutrinoless double beta decay observes the Majorana neutrino mass. Electron capture e. g. on 163Ho plus bound electron to 163Dy* plus neutrino can determine the electron neutrino mass from the upper end of the decay spectrum of the excited Dy*, which is given by the Q-Value minus the neutrino mass. The Dy* states decay by X-ray and Auger electron emissions. The total decay energy is measured in a bolometer. These excitations have been studied by Robertson and by Faessler et al.. In addition the daughter atom Dy can also be excited by moving in the capture process one electron into the continuum. The escape of these continuum electrons is automatically included in the experimental bolometer spectrum. Recently a method developed by Intemann and Pollock was used by DeRujula and Lusignoli for a rough estimate of this shake-off process for "s" wave electrons in capture on 163H...

  8. Low mass stellar evolution with WIMP capture and annihilation

    CERN Document Server

    Scott, Pat; Fairbairn, Malcolm

    2007-01-01

    Recent work has indicated that WIMP annihilation in stellar cores has the potential to contribute significantly to a star's total energy production. We report on progress in simulating the effects of WIMP capture and annihilation upon stellar structure and evolution near supermassive black holes, using the new DarkStars code. Preliminary results indicate that low-mass stars are the most influenced by WIMP annihilation, which could have consequences for upcoming observational programs.

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

    Energy Technology Data Exchange (ETDEWEB)

    Fairchild, R.G.; Bond, V.P.

    1982-01-01

    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 /sup 10/B(n,..cap alpha..)/sup 7/Li reaction is approx. 10 ..mu..m, 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. (ERB)

  10. 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

  11. 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

  12. 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.

  13. 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

  14. 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

  15. Mass spectrometry for determination of bioactive compounds

    Digital Repository Service at National Institute of Oceanography (India)

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

    are naturally occurring nitrogen containing biologically active heterocyclic compounds. Over the last few years, a large number of biologically important alkaloids with antiviral, antibacterial, anti- inflammatory, antimalarial, antioxidant and anticancer...

  16. 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

  17. 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.

  18. 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.

  19. 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

  20. 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

  1. 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

  2. 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.

  3. 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.

  4. 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

  5. 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)

  6. 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.

  7. 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 ...

  8. 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

  9. 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

  10. 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

  11. 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.)

  12. 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...

  13. 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.

  14. 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...

  15. 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

  16. 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.

  17. 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

  18. 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...

  19. 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.

  20. GRACE captures basin mass dynamic changes in China based on a multi-basin inversion method

    Science.gov (United States)

    Yi, Shuang; Wang, Qiuyu; Sun, Wenke

    2016-04-01

    Complex landform, miscellaneous climate and enormous population have enriched China with geophysical phenomena ranging from water depletion in the underground to glaciers retreat on the high mountains and have aroused large scientific interests. This paper, utilizing gravity observations 2003-2014 from the Gravity Recovery and Climate Experiment (GRACE), intends to make a comprehensive estimation of mass status in 16 drainage basins in the whole region. We proposed a multi-basin inversion method, which is featured by resistance to the stripe noise and ability to alleviate signal attenuation due to truncation and smoothing of GRACE data. The results show both positive and negative trends: there is a tremendous mass accumulation spreading from the Tibetan plateau (12.2 ± 0.6 Gt/yr) to the Yangtze River (7.6 ± 1.3 Gt/yr), and further to the southeast coastal areas, which is suggested to involve an increase in the ground water storage, lake and reservoir water volume and likely materials flowed in by tectonic process; a mass loss is occurring in Huang-Huai-Hai-Liao River Basin (-10.5 ± 0.8 Gt/yr), as well as the Brahmaputra-Nujiang-Lancang River Basin (-15.0 ± 0.9 Gt/yr) and Tienshan Mountain (-4.1 ± 0.3 Gt/yr), which is a result of groundwater pumping and glacier melting. The groundwater depletion area is well consistent with the distribution of land subsidence in North China. In the end, we find intensified precipitation can alter the local water supply and GRACE is proficient to capture this dynamics, which could be instructive for the South-to-North Water Diversion - one China's giant hydrologic project.

  1. 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

  2. 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

  3. 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.

  4. 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.

  5. 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.

  6. Mass measurements of neutron rich isotopes in the Fe region and electron capture processes in neutron star crusts

    Energy Technology Data Exchange (ETDEWEB)

    Estrade, Alfredo [National Superconducting Cyclotron Laboratory (NSCL); Matos, M. [Louisiana State University; Schatz, Hendrik [Michigan State University, East Lansing; Amthor, A. M. [National Superconducting Cyclotron Laboratory (NSCL); Beard, Mary [University of Notre Dame, IN; Brown, Edward [Michigan State University, East Lansing; Bazin, D. [National Superconducting Cyclotron Laboratory (NSCL); Becerril, A. [National Superconducting Cyclotron Laboratory (NSCL); Elliot, T [National Superconducting Cyclotron Laboratory (NSCL); Gade, A. [National Superconducting Cyclotron Laboratory (NSCL); Galaviz, D. [National Superconducting Cyclotron Laboratory (NSCL); Gupta, Sanjib [Indian Institute of Technology, Kanpur; Hix, William Raphael [ORNL; Lau, Rita [National Superconducting Cyclotron Laboratory (NSCL); Moeller, Peter [Los Alamos National Laboratory (LANL); Pereira, J. [National Superconducting Cyclotron Laboratory (NSCL); Portillo, M. [National Superconducting Cyclotron Laboratory (NSCL); Rogers, A. M. [National Superconducting Cyclotron Laboratory (NSCL); Shapira, Dan [ORNL; Smith, E. [Ohio State University; Stolz, A. [Michigan State University, East Lansing; Wallace, M. [Los Alamos National Laboratory (LANL); Wiescher, Michael [University of Notre Dame, IN

    2010-01-01

    Experimental knowledge of nuclear masses of exotic nuclei is important for understanding nu- clear structure far from the valley of -stability, and as a direct input into astrophysical models. Electron capture processes in the crust of accreting neutron stars have been proposed as a heat source that can affect the thermal structure of the star. Nuclear masses of very neutron-rich nu- clides are necessary inputs to model the electron capture process. The time-of-flight (TOF) mass measurement technique allows measurements on very short-lived nuclei. It has been effectively applied using the fast fragment beams produced at the National Superconducting Cyclotron Lab (NSCL) to reach masses very far from stability. Measurements were performed for neutron-rich isotopes in the region of the N=32 and N=40 subshells, which coincides with the mass range of carbon superburst ashes. We discuss reaction network calculations performed to investigate the impact of our new measurements and to compare the effect of using different global mass models in the calculations. It is observed that the process is sensitive to the differences in the odd-even mass staggering predicted by the mass models, and our new result for 66Mn has a significant impact on the distribution of heat sources in the crust.

  7. The capture of dark matter particles through the evolution of low-mass stars

    CERN Document Server

    Lopes, Ilídio; Eugénio, Daniel

    2011-01-01

    We studied the rate at which stars capture dark matter (DM) particles, considering different assumptions regarding the DM characteristics and in particular investigating how the stellar physics influences the capture rate. Two scenarios were considered: firstly, we assumed the maximal values for the spin-dependent and spin-independent DM particle-nucleon scattering cross sections allowed by the limits from direct detection experiments. Secondly, we considered that both scattering cross sections are of the same order, with the aim of studying the dependencies of the capture rate on stellar elements other than hydrogen. We found that the characteristics of the capture rate are very different in the two scenarios. Furthermore, we quantified the uncertainties on the computed capture rate (C_x) and on the ratio between the luminosities from DM annihilations and thermonuclear reactions (L_x/L_nuc) derived from an unprecise knowledge of the stellar structure and DM parameters. For instance, while an uncertainty of 1...

  8. -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.

  9. 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...

  10. 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...

  11. 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...

  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. Thermokinetic/mass-transfer analysis of carbon capture for reuse/sequestration.

    Energy Technology Data Exchange (ETDEWEB)

    Stechel, Ellen Beth; Brady, Patrick Vane; Staiger, Chad Lynn; Luketa, Anay Josephine

    2010-09-01

    Effective capture of atmospheric carbon is a key bottleneck preventing non bio-based, carbon-neutral production of synthetic liquid hydrocarbon fuels using CO{sub 2} as the carbon feedstock. Here we outline the boundary conditions of atmospheric carbon capture for recycle to liquid hydrocarbon fuels production and re-use options and we also identify the technical advances that must be made for such a process to become technically and commercially viable at scale. While conversion of atmospheric CO{sub 2} into a pure feedstock for hydrocarbon fuels synthesis is presently feasible at the bench-scale - albeit at high cost energetically and economically - the methods and materials needed to concentrate large amounts of CO{sub 2} at low cost and high efficiency remain technically immature. Industrial-scale capture must entail: (1) Processing of large volumes of air through an effective CO{sub 2} capture media and (2) Efficient separation of CO{sub 2} from the processed air flow into a pure stream of CO{sub 2}.

  15. 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

  16. A mass-spectroscopic analysis of the sulfurous compounds in average fractions of Romashkin oils

    Energy Technology Data Exchange (ETDEWEB)

    Kubas, M.; Kubelka, V.; Mostecky, J.; Vodicka, L.

    1982-01-01

    Results are presented of an analysis of sulfurous compounds in an average fraction of Romashkin (USSR) oils, produced by the method of mass-spectrometry. Some individual properties of the benzothiophene type were determined. It is shown, that in the average distillate of Romashkin petroleum, benzothiophenes are dominant.

  17. 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...

  18. 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.

  19. 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

    2016-08-30

    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.

  20. 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

  1. 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

  2. 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).

  3. 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

  4. 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.

  5. 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.

  6. Electron Capture Dissociation of Sodium-Adducted Peptides on a Modified Quadrupole/Time-of-Flight Mass Spectrometer

    Science.gov (United States)

    Voinov, Valery G.; Hoffman, Peter D.; Bennett, Samuel E.; Beckman, Joseph S.; Barofsky, Douglas F.

    2015-12-01

    Electron capture dissociation (ECD), which generally preserves the position of labile post-translational modifications, can be a powerful method for de novo sequencing of proteins and peptides. In this report, ECD product-ion mass spectra of singly and doubly sodiated, nonphosphorylated, and phosphorylated peptides are presented and compared with the ECD mass spectra of their protonated counterparts. ECD of doubly charged, singly sodiated peptides yielded essentially the same sequence information as was produced by the corresponding doubly protonated peptides. The presence of several sodium binding sites on the polypeptide backbone, however, resulted in more complicated spectra. This situation is aggravated by the zwitterionic equilibrium of the free acid peptide precursors. The product-ion spectra of doubly and triply charged peptides possessing two sodium ions were further complicated by the existence of isomers created by the differential distribution of sodium binding sites. Triply charged, phosphorylated precursors containing one sodium, wherein the sodium is attached exclusively to the PO4 group, were found to be as useful for sequence analysis as the fully protonated species. Although sodium adducts are generally minimized during sample preparation, it appears that they can nonetheless provide useful sequence information. Additionally, they enable straightforward identification of a peptide's charge state, even on low-resolution instruments. The experiments were carried out using a radio frequency-free electromagnetostatic cell retrofitted into the collision-induced dissociation (CID) section of a hybrid quadrupole/time-of-flight tandem mass spectrometer.

  7. 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

  8. 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

  9. 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.

  10. 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

  11. Low-molecular-mass thiol compounds from a free-living highly pathogenic amoeba, Naegleria fowleri.

    Science.gov (United States)

    Ondarza, Raúl N; Iturbe, Angélica; Hernández, Eva; Hurtado, Gerardo

    2003-04-01

    Acid extracts labelled with the fluorescent reagent monobromobimane and separated by HPLC have enabled the detection of low-molecular-mass thiol compounds in Naegleria fowleri for the first time. The amounts detected are expressed in nmol/1 x 10(6) trophozoites cultivated at various stages of growth in the appropriate culture medium. N. fowleri is a highly pathogenic free-living amoeba, in which we found important thiol compounds, some of them in their reduced and oxidized forms. Unlike cysteine and glutathione, a number of these are not represented in normal human lymphocytes. Some of these thiol compounds from Naegleria must have their respective disulphide reductases, although the presence of thiol-disulphide exchange reactions must be considered. Ovothiol A, with antioxidant properties, is an example of a compound that is kept reduced by trypanothione in trypanosomatids, although no disulphide reductase for ovothiol A has yet been discovered. In our case we were unable to detect this biothiol in Naegleria. The presence of thiol compounds that seem to be particular to this pathogen and which are not present in human lymphocytes opens the possibility of searching for disulphide-reducing enzymes that can serve as drug targets.

  12. 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.

  13. 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.

  14. Mapping a Noncovalent Protein-Peptide Interface by Top-Down FTICR Mass Spectrometry Using Electron Capture Dissociation

    Science.gov (United States)

    Clarke, David J.; Murray, Euan; Hupp, Ted; Mackay, C. Logan; Langridge-Smith, Pat R. R.

    2011-08-01

    Noncovalent protein-ligand and protein-protein complexes are readily detected using electrospray ionization mass spectrometry (ESI MS). Furthermore, recent reports have demonstrated that careful use of electron capture dissociation (ECD) fragmentation allows covalent backbone bonds of protein complexes to be dissociated without disruption of noncovalent protein-ligand interactions. In this way the site of protein-ligand interfaces can be identified. To date, protein-ligand complexes, which have proven tractable to this technique, have been mediated by ionic electrostatic interactions, i.e., ion pair interactions or salt bridging. Here we extend this methodology by applying ECD to study a protein-peptide complex that contains no electrostatics interactions. We analyzed the complex between the 21 kDa p53-inhibitor protein anterior gradient-2 and its hexapeptide binding ligand (PTTIYY). ECD fragmentation of the 1:1 complex occurs with retention of protein-peptide binding and analysis of the resulting fragments allows the binding interface to be localized to a C-terminal region between residues 109 and 175. These finding are supported by a solution-phase competition assay, which implicates the region between residues 108 and 122 within AGR2 as the PTTIYY binding interface. Our study expands previous findings by demonstrating that top-down ECD mass spectrometry can be used to determine directly the sites of peptide-protein interfaces. This highlights the growing potential of using ECD and related top-down fragmentation techniques for interrogation of protein-protein interfaces.

  15. 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.

  16. Lichen specific thallus mass and secondary compounds change across a retrogressive fire-driven chronosequence.

    Directory of Open Access Journals (Sweden)

    Johan Asplund

    Full Text Available In the long-term absence of major disturbances ecosystems enter a state of retrogression, which involves declining soil fertility and consequently a reduction in decomposition rates. Recent studies have looked at how plant traits such as specific leaf mass and amounts of secondary compounds respond to declining soil fertility during retrogression, but there are no comparable studies for lichen traits despite increasing recognition of the role that lichens can play in ecosystem processes. We studied a group of 30 forested islands in northern Sweden differing greatly in fire history, and collectively representing a retrogressive chronosequence, spanning 5000 years. We used this system to explore how specific thallus mass (STM and carbon based secondary compounds (CBSCs change in three common epiphytic lichen species (Hypogymnia phsyodes, Melanohalea olivacea and Parmelia sulcata as soil fertility declines during this retrogression. We found that STMs of lichens increased sharply during retrogression, and for all species soil N to P ratio (which increased during retrogression was a strong predictor of STM. When expressed per unit area, medullary CBSCs in all species and cortical CBSCs in P. sulcata increased during retrogression. Meanwhile, when expressed per unit mass, only cortical CBSCs in H. physodes responded to retrogression, and in the opposite direction. Given that lichen functional traits are likely to be important in driving ecological processes that drive nutrient and carbon cycling in the way that plant functional traits are, the changes that they undergo during retrogression could potentially be significant for the functioning of the ecosystem.

  17. Enhanced Volatile Organic Compounds emissions and organic aerosol mass increase the oligomer content of atmospheric aerosols

    Science.gov (United States)

    Kourtchev, Ivan; Giorio, Chiara; Manninen, Antti; Wilson, Eoin; Mahon, Brendan; Aalto, Juho; Kajos, Maija; Venables, Dean; Ruuskanen, Taina; Levula, Janne; Loponen, Matti; Connors, Sarah; Harris, Neil; Zhao, Defeng; Kiendler-Scharr, Astrid; Mentel, Thomas; Rudich, Yinon; Hallquist, Mattias; Doussin, Jean-Francois; Maenhaut, Willy; Bäck, Jaana; Petäjä, Tuukka; Wenger, John; Kulmala, Markku; Kalberer, Markus

    2016-10-01

    Secondary organic aerosol (SOA) accounts for a dominant fraction of the submicron atmospheric particle mass, but knowledge of the formation, composition and climate effects of SOA is incomplete and limits our understanding of overall aerosol effects in the atmosphere. Organic oligomers were discovered as dominant components in SOA over a decade ago in laboratory experiments and have since been proposed to play a dominant role in many aerosol processes. However, it remains unclear whether oligomers are relevant under ambient atmospheric conditions because they are often not clearly observed in field samples. Here we resolve this long-standing discrepancy by showing that elevated SOA mass is one of the key drivers of oligomer formation in the ambient atmosphere and laboratory experiments. We show for the first time that a specific organic compound class in aerosols, oligomers, is strongly correlated with cloud condensation nuclei (CCN) activities of SOA particles. These findings might have important implications for future climate scenarios where increased temperatures cause higher biogenic volatile organic compound (VOC) emissions, which in turn lead to higher SOA mass formation and significant changes in SOA composition. Such processes would need to be considered in climate models for a realistic representation of future aerosol-climate-biosphere feedbacks.

  18. Mass spectrometry investigation of Titan aerosols analogs formed with traces of aromatic compounds

    Science.gov (United States)

    Gautier, Thomas; Trainer, Melissa; Sebree, Joshua; Li, Xiang; Pinnick, Veronica; Getty, Stephanie; Brinckerhoff, Will

    2016-06-01

    The detection of benzene at ppm levels in Titan's atmosphere [1] by Cassini's Ion and Neutral Mass Spectrometer (INMS) supports the idea that aromatic and heteroaromatic reaction pathways may play an important role in Titan's aerosols formation. In laboratory studies it has been shown that these aromatic molecules are easily dissociated by ultraviolet radiation and can therefore contribute significantly to aerosol formation [2] and be used to dope the production of aerosol analogs [3]. In this work we investigate the effect on the aerosol composition and growth pattern of the chemical nature of the aromatic reactant used to produce aerosol. Analysis are performed using Laser Desorption-Time of Flight mass spectrometry (LD-TOF) and Fourier Transform Infrared Spectroscopy (FTIR) Infrared analysis of our samples shows that inclusion of aromatic compounds as trace precursors allows to better fit laboratory data to Titan aerosol spectra observed by Cassini [3,4]. The improvement is especially visible on the far infrared (˜200 cm-1) bands observed by CIRS [5]. LDMS results show that the aerosol growth patterns depend both on the number of rings and on the nitrogen content of the trace precursor used. We also perform MS/MS analysis on some prominent peaks of aerosol mass spectra. This MS/MS approach allows us to identify some of the key compounds in the aerosol growth processes.

  19. Evaluation of column hardware on liquid chromatography-mass spectrometry of phosphorylated compounds.

    Science.gov (United States)

    Sakamaki, Hiroshi; Uchida, Takeharu; Lim, Lee Wah; Takeuchi, Toyohide

    2015-02-13

    The influences of column hardware, such as chromatographic tubes and frits, on liquid chromatography-mass spectrometry (LC-MS) analysis of phosphorylated compounds were evaluated. The signal to noise ratio (S/N) and the intensity of flavin adenine dinucleotide (FAD) using a glass lined tube and polyethylene frit (GL-PE) column was approximately 170 and 90 times higher, respectively, than those using conventional stainless steel tube and stainless steel frit (S-S) column. In addition, the retention time of FAD using GL-PE column was the shortest compared to other columns. Interaction between phosphorylated compounds and metal ions in the flow path in the S-S column was stronger than that between them and the GL-PE column. Thus, the metal ions in the flow path in GL-PE column were low. Since the specific surface area of a pair of frits was 70 times larger than that of a chromatographic tube (150 mm×2.1 mm), the frits were found to have more effective improvement of the S/N as well as the intensity than the chromatographic tubes, when phosphorylated compounds were analyzed by LC-MS. When the evaluated phosphorylated compounds were analyzed by LC-MS(/MS) using a GL-PE column, the intensity and S/N were increased.

  20. 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

  1. 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.

  2. Identification of compounds in wine by HPLC-tandem mass spectrometry.

    Science.gov (United States)

    Bevilacqua, Lucio; Buiarelli, Francesca; Coccioli, Franco; Jasionowska, Renata

    2004-01-01

    In this work several compounds were detected in wines by HPLC-tandem mass spectrometry. In particular cinnamic and benzoic acids, tyrosol, apigenin-7-glucoside and luteolin-7-glucoside were identified and quantified in Italian wines. Red wines show bigger amount of cinnamic and benzoic acids than white wines. tyrosol is in bigger amount with respect to two flavones: luteolin-7-glucoside and apigenin-7-glucoside. These last two flavones are only in some wine, but it can be important to detect the presence of different substances in small amount to be able to characterize a wine. PMID:15506618

  3. Capturing the crystal: prediction of enthalpy of sublimation, crystal lattice energy, and melting points of organic compounds.

    Science.gov (United States)

    Salahinejad, Maryam; Le, Tu C; Winkler, David A

    2013-01-28

    Accurate computational prediction of melting points and aqueous solubilities of organic compounds would be very useful but is notoriously difficult. Predicting the lattice energies of compounds is key to understanding and predicting their melting behavior and ultimately their solubility behavior. We report robust, predictive, quantitative structure-property relationship (QSPR) models for enthalpies of sublimation, crystal lattice energies, and melting points for a very large and structurally diverse set of small organic compounds. Sparse Bayesian feature selection and machine learning methods were employed to select the most relevant molecular descriptors for the model and to generate parsimonious quantitative models. The final enthalpy of sublimation model is a four-parameter multilinear equation that has an r(2) value of 0.96 and an average absolute error of 7.9 ± 0.3 kJ.mol(-1). The melting point model can predict this property with a standard error of 45° ± 1 K and r(2) value of 0.79. Given the size and diversity of the training data, these conceptually transparent and accurate models can be used to predict sublimation enthalpy, lattice energy, and melting points of organic compounds in general.

  4. 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.

  5. In-Situ Organic Compound Analysis of the Meteorite Surface by Desorption Electrospray Ionization Coupled with an Orbitrap Mass Spectrometer

    Science.gov (United States)

    Naraoka, H.; Hashiguchi, M.

    2016-08-01

    It-situ analysis of organic compounds on the meteorite surface was performed by desorption electrospray ionization coupled with high resolution mass spectrometry. Indigenous peaks of meteorite origin were discriminated from the background.

  6. Molecular simulation studies of CO2 adsorption by carbon model compounds for carbon capture and sequestration applications.

    Science.gov (United States)

    Liu, Yangyang; Wilcox, Jennifer

    2013-01-01

    Effects of oxygen-containing surface functionalities on the adsorption of mixtures including CO(2)/CH(4), CO(2)/N(2), and CO(2)/H(2)O have been investigated in the current work. Together with Bader charge analysis, electronic structure calculations have provided the initial framework comprising both the geometry and corresponding charge information required to carry out statistical-based molecular simulations. The adsorption isotherms and selectivity of CO(2) from CO(2)/N(2), CO(2)/CH(4), and CO(2)/H(2)O gas mixtures were determined by grand canonical Monte Carlo simulations at temperature/pressure conditions relevant to carbon capture and sequestration applications. The interactions between the surfaces with induced polarity and nonpolar/polar molecules have been investigated. It has been observed that, due to the induced polarity of the surface functionalization, the selectivity of CO(2) over CH(4) increases from approximately 2 to higher than 5, and the selectivity of CO(2) over N(2) increases from approximately 5 to 20, especially in the low-pressure regime. However, water vapor will always preferentially adsorb over CO(2) in carbon-based systems containing oxygen functionalized surfaces at conditions relevant to carbon capture application. Molecular simulation results indicate that the surface chemistry in micropores is tunable thereby influencing the selectivity for enhanced uptake of CO(2).

  7. 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.

  8. 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

    capture dissociation (ECD) of peptide ions provides protein identification. When a measured peptide molecular mass indicates the possibility of a PTM, vibrational excitation is applied to determine via characteristic losses the type and eventually the structure of the modification, while ECD determines...

  9. 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...

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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

  15. 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.)

  16. 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

  17. 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

  18. 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.

  19. Analysis of volatile and oxidation sensitive compounds using a cold inlet system and electron impact mass spectrometry.

    Science.gov (United States)

    Sproß, Jens

    2014-09-05

    This video presents a protocol for the mass spectrometrical analysis of volatile and oxidation sensitive compounds using electron impact ionization. The analysis of volatile and oxidation sensitive compounds by mass spectrometry is not easily achieved, as all state-of-the-art mass spectrometric methods require at least one sample preparation step, e.g., dissolution and dilution of the analyte (electrospray ionization), co-crystallization of the analyte with a matrix compound (matrix-assisted laser desorption/ionization), or transfer of the prepared samples into the ionization source of the mass spectrometer, to be conducted under atmospheric conditions. Here, the use of a sample inlet system is described which enables the analysis of volatile metal organyls, silanes, and phosphanes using a sector field mass spectrometer equipped with an electron impact ionization source. All sample preparation steps and the sample introduction into the ion source of the mass spectrometer take place either under air-free conditions or under vacuum, enabling the analysis of compounds highly susceptible to oxidation. The presented technique is especially of interest for inorganic chemists, working with metal organyls, silanes, or phosphanes, which have to be handled using inert conditions, such as the Schlenk technique. The principle of operation is presented in this video.

  20. 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...

  1. 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

  2. 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

  3. 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.

  4. Sub-parts-per-billion determination of nitro-substituted polynuclear aromatic hydrocarbons in airborne particulate matter and soil by electron capture-Tandem mass spectrometry.

    Science.gov (United States)

    Vincenti, M; Minero, C; Pelizzetti, E; Fontana, M; De Maria, R

    1996-12-01

    A procedure for the determination of nitro-substiruted polynuclear aromatic hydrocarbons (nitro-PAH) on crude air-particulate and soil extracts is introduced. Elimination of purification and fractionation procedures was made possible by the use of both a selective ionization method, such as electron-capture chemical ionization, and a specific fragmentation process, in an experiment of tandem mass spectrometry (gas chromatography-electron capture tandem mass spectrometry). Different mass spectrometric procedures were compared. The best performance was observed when the nitro-PAH molecular ions [M](-) were mass-selected by the first analyzer under multiple reaction monitoring conditions and then fragmented to NO 2 (-) (m/z 46). Detection limits were on the order of hundreds of femtograms, as determined in extracts of real environmental samples. This corresponds approximately to 5-15 pg of nitro-PAH per cubic meter of air sampled. Calibration curves were linear over 3 orders of magnitude. Applications to contamination from motor vehicle combustion and the iron industry are briefly discussed.

  5. 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

  6. 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

  7. 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...

  8. 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...

  9. 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.)

  10. 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

  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

    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.)

  12. 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

  13. 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)

  14. 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

  15. 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

  16. 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

  17. 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.

  18. Determination of heat purgeable and ambient purgeable volatile organic compounds in water by gas chromatography/mass spectrometry

    Science.gov (United States)

    Rose, Donna L.; Sandstrom, Mark W.; Murtagh, Lucinda K.

    2016-09-08

    Two new analytical methods have been developed by the U.S. Geological Survey (USGS) National Water Quality Laboratory (NWQL) that allow the determination of 37 heat purgeable volatile organic compounds (VOCs) (USGS Method O-4437-16 [NWQL Laboratory Schedule (LS) 4437]) and 49 ambient purgeable VOCs (USGS Method O-4436-16 [NWQL LS 4436]) in unfiltered water. This report documents the procedures and initial performance of both methods. The compounds chosen for inclusion in the methods were determined as having high priority by the USGS National Water-Quality Assessment (NAWQA) Program. Both methods use a purge-and-trap technique with gas chromatography/mass spectrometry. The compounds are extracted from the sample by bubbling helium through a 25-milliliter sample. For the polar and less volatile compounds, the sample is heated at 60 degrees Celsius, whereas the less polar and more volatile compounds are purged using a separate analytical procedure at ambient temperature. The compounds are trapped on a sorbent trap, desorbed into a gas chromatograph/mass spectrometer for separation, and then identified and quantified. Sample preservation is recommended for both methods by adding a 1:1 solution of hydrochloric acid (HCl [1:1]) to water samples to adjust the pH to 2. Analysis within 14 days from sampling is recommended.The heat purgeable method (USGS Method O-4437-16) operates with the mass spectrometer in the simultaneous full scan/selected ion monitoring mode. This method supersedes USGS Method O-4024-03 (NWQL LS 4024). Method detection limits (MDLs) for fumigant compounds 1,2-dibromoethane, 1,2-dichloropropane, 1,2,3-trichloropropane, chloropicrin, and 1,2-dibromo-3-chloropropane range from 0.002 to 0.010 microgram per liter (µg/L). The MDLs for all remaining heat purgeable VOCs range from 0.006 µg/L for tert-butyl methyl ether to 3 µg/L for alpha-terpineol. Calculated holding times indicate that 36 of the 37 heat purgeable VOCs are stable for a minimum of 14 days

  19. Optimization and Application of APCI Hydrogen-Deuterium Exchange Mass Spectrometry (HDX MS) for the Speciation of Nitrogen Compounds.

    Science.gov (United States)

    Acter, Thamina; Cho, Yunju; Kim, Sungji; Ahmed, Arif; Kim, Byungjoo; Kim, Sunghwan

    2015-09-01

    A systematic study was performed to investigate the utility of atmospheric pressure chemical ionization hydrogen-deuterium exchange mass spectrometry (APCI HDX MS) to identify the structures of nitrogen-containing aromatic compounds. First, experiments were performed to determine the optimized experimental conditions, with dichloromethane and CH(3)OD found to be good cosolvents for APCI HDX. In addition, a positive correlation between the heated capillary temperature and the observed HDX signal was observed, and it was suggested that the HDX reaction occurred when molecules were contained in the solvent cluster. Second, 20 standard nitrogen-containing compounds were analyzed to investigate whether speciation could be determined based on the different types of ions produced from nitrogen-containing compounds with various functional groups. The number of exchanges occurring within the compounds correlated well with the number of active hydrogen atoms attached to nitrogen, and it was confirmed that APCI HDX MS could be used to determine speciation. The results obtained by APCI HDX MS were combined with the subsequent investigation of the double bond equivalence distribution and indicated that resins of shale oil extract contained mostly pyridine type nitrogen compounds. This study confirmed that APCI HDX MS can be added to previously reported chemical ionization, electrospray ionization, and atmospheric pressure photo ionization-based HDX methods, which can be used for structural elucidation by mass spectrometry.

  20. 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.

  1. 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

  2. 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...

  3. 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

  4. 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.

  5. 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. ...

  6. 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...

  7. Comment on "Organics captured from comet 81P/Wild 2 by the Stardust spacecraft".

    Science.gov (United States)

    Spencer, Maegan K; Zare, Richard N

    2007-09-21

    Sandford et al. (Reports, 15 December 2006, p. 1720) reported on organic compounds captured from Comet 81P/Wild 2 by the Stardust spacecraft. We emphasize the difficulty in assigning the origin of compounds detected diffusely along particle impact tracks and show that rapid heating of aerogel that has never been exposed to cometary particle capture can generate complex aromatic molecules from low-mass carbon impurities present in the aerogel.

  8. Detection of volatile compounds produced by microbial growth in urine by selected ion flow tube mass spectrometry (SIFT-MS).

    Science.gov (United States)

    Storer, Malina K; Hibbard-Melles, Kim; Davis, Brett; Scotter, Jenny

    2011-10-01

    Selected ion flow tube-mass spectrometry has been used to measure the volatile compounds occurring in the headspace of urine samples inoculated with common urinary tract infection (UTI)-causing microbes Escherichia coli, Proteus vulgaris, Pseudomonas aeruginosa, Staphylococcus aureus, Staphylococcus epidermidis, Klebsiella pneumoniae, Enterococcus faecalis, or Candida albicans. This technique has the potential to offer rapid and simple diagnosis of the causative agent of UTIs.

  9. Emissions of volatile organic compounds from Quercus ilex L. measured by Proton Transfer Reaction Mass Spectrometry under different environmental conditions

    Science.gov (United States)

    Holzinger, R.; Sandoval-Soto, L.; Rottenberger, S.; Crutzen, P. J.; Kesselmeier, J.

    2000-08-01

    Volatile organic compound (VOC) emissions of the Mediterranean holm oak (Quercus ilex L.) were investigated using a fast Proton Transfer Reaction Mass Spectrometry (PTR-MS) instrument for analysis. This technique is able to measure compounds with a proton affinity higher than water with a high time resolution of 1 s per compound. Hence nearly all VOCs can be detected on-line. We could clearly identify the emission of methanol, acetaldehyde, ethanol, acetone, acetic acid, isoprene, monoterpenes, toluene, and C10-benzenes. Some other species could be tentatively denominated. Among these are the masses 67 (cyclo pentadiene), mass 71 (tentatively attributed to methyl vinyl ketone (MVK) and metacrolein (MACR)), 73 (attributed to methyl ethyl ketone (MEK)), 85 (C6H12 or hexanol), and 95 (vinylfuran or phenol). The emissions of all these compounds (identified as well as nonidentified) together represent 99% of all masses detected and account for a carbon loss of 0.7-2.9% of the net photosynthesis. Of special interest was a change in the emission behavior under changing environmental conditions such as flooding or fast light/dark changes. Flooding of the root system caused an increase of several VOCs between 60 and 2000%, dominated by the emission of ethanol and acetaldehyde, which can be explained by the well described production of ethanol under anoxic conditions of the root system and the recently described subsequent transport and partial oxidation to acetaldehyde within the green leaves. However, ethanol emissions were dominant. Additionally, bursts of acetaldehyde with lower ethanol emission were also found under fast light/dark changes. These bursts are not understood.

  10. 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\

  11. 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.

  12. 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...

  13. 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

  14. 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.

  15. 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)

  16. 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

  17. 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...

  18. 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

  19. Search for neutrinos from annihilation of captured low-mass dark matter particles in the sun by super-kamiokande.

    Science.gov (United States)

    Choi, K; 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, T; Kametani, I; Kaneyuki, K; Lee, K P; Nishimura, Y; Okumura, K; McLachlan, T; Labarga, L; Kearns, E; Raaf, J L; Stone, J L; Sulak, L R; Berkman, S; Tanaka, H A; Tobayama, 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; Martens, K; Marti, Ll; Vagins, M R; Martin, J F; de Perio, P; Konaka, A; Wilking, M J; Chen, S; Zhang, Y; Wilkes, R J

    2015-04-10

    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}-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 WIMP-proton cross section for WIMP masses below 200  GeV/c^{2} (at 10  GeV/c^{2}, 1.49×10^{-39}  cm^{2} for χχ→bb[over ¯] and 1.31×10^{-40}  cm^{2} for χχ→τ^{+}τ^{-} annihilation channels), also ruling out some fraction of WIMP candidates with spin-independent coupling in the few-GeV/c^{2} mass range. PMID:25910107

  20. Mass spectrometry-based sequencing of protein C-terminal peptide using α-carboxyl group-specific derivatization and COOH capturing.

    Science.gov (United States)

    Nakajima, Chihiro; Kuyama, Hiroki; Tanaka, Koichi

    2012-09-15

    An approach to mass spectrometry (MS)-based sequence analysis of selectively enriched C-terminal peptide from protein is described. This approach employs a combination of the specific derivatization of α-carboxyl group (α-COOH), enzymatic proteolysis using endoproteinase GluC, and enrichment of C-terminal peptide through the use of COOH-capturing material. Highly selective derivatization of α-COOH was achieved by a combination of specific activation of α-COOH through oxazolone chemistry and amidation using 3-aminopropyltris-(2,4,6-trimethoxyphenyl)phosphonium bromide (TMPP-propylamine). This amine component was used to simplify fragmentation in tandem mass spectrometry (MS/MS) measurement, which facilitated manual sequence interpretation. The peptides produced after GluC digestion were then treated with a COOH scavenger to enrich the C-terminal peptide that is only devoid of COOH groups, and the obtained C-terminal peptide was readily sequenced by matrix-assisted laser desorption/ionization (MALDI)-MS/MS due to the TMPP mass tag.

  1. 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...

  2. 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...

  3. 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

  4. Mass spectrometry and /sup 13/C nuclear magnetic resonance spectroscopy of compounds modeling the glycopeptide linkage of glycoproteins

    Energy Technology Data Exchange (ETDEWEB)

    Blumberg, K.; Bush, C.A.

    1982-01-15

    The properties of several compounds useful as models for three-dimensional conformational studies and the investigation of the chemical degradation of glycopeptide linkages both of the N- and O-glycosidic type are described. Using the method of differential chemical shift in H/sub 2/O and D/sub 2/O as solvents, the carbon NMR spectrum of N-acetylglucosaminylasparagine, 1-N-acetyl-..beta..-D-glucopyranosylamine, and 1-N-acetyl-2-acetamido-..beta..-D-glycopyranosylamine has been assigned. Electron impact mass spectra of the peracetylated derivatives of the latter two compounds show a peak apparently unique to glycopyranosylamides at m/e = 269, no analog of which is observed in the mass spectra of other peracetylated sugars. As models of the ..cap alpha..-O-glycosidic linkage, fully assigned carbon NMR spectra of ..cap alpha..-methyl-N-acetylgalactosamine (GalNAc), ..cap alpha..-methyl-3-O-methyl GalNAc, and -GlcNAc as well as the disaccharide Glc-..beta..-l ..-->.. 3 GalNAc are reported. Because certain anomalies in the chemical shifts and /sup 1/J/sub CH/ observed in the disaccharide and in O-glycosylated glycoproteins are not observed in the simple model compounds, they may result from conformational interactions in the glycopeptides.

  5. 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.

  6. Potential of needle trap microextraction-portable gas chromatography-mass spectrometry for measurement of atmospheric volatile compounds

    Science.gov (United States)

    Feijó Barreira, Luís Miguel; Xue, Yu; Duporté, Geoffroy; Parshintsev, Jevgeni; Hartonen, Kari; Jussila, Matti; Kulmala, Markku; Riekkola, Marja-Liisa

    2016-08-01

    Volatile organic compounds (VOCs) play a key role in atmospheric chemistry and physics. They participate in photochemical reactions in the atmosphere, which have direct implications on climate through, e.g. aerosol particle formation. Forests are important sources of VOCs, and the limited resources and infrastructures often found in many remote environments call for the development of portable devices. In this research, the potential of needle trap microextraction and portable gas chromatography-mass spectrometry for the study of VOCs at forest site was evaluated. Measurements were performed in summer and autumn 2014 at the Station for Measuring Ecosystem-Atmosphere Relations (SMEAR II) in Hyytiälä, Finland. During the first part of the campaign (summer) the applicability of the developed method was tested for the determination of monoterpenes, pinonaldehyde, aldehydes, amines and anthropogenic compounds. The temporal variation of aerosol precursors was determined, and evaluated against temperature and aerosol number concentration data. The most abundant monoterpenes, pinonaldehyde and aldehydes were successfully measured, their relative amounts being lower during days when particle number concentration was higher. Ethylbenzene, p- and m-xylene were also found when wind direction was from cities with substantial anthropogenic activity. An accumulation of VOCs in the snow cover was observed in the autumn campaign. Results demonstrated the successful applicability of needle trap microextraction and portable gas chromatography-mass spectrometry for the rapid in situ determination of organic gaseous compounds in the atmosphere.

  7. 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)

  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. A novel immuno-competitive capture mass spectrometry strategy for protein-protein interaction profiling reveals that LATS kinases regulate HCV replication through NS5A phosphorylation.

    Science.gov (United States)

    Meistermann, Hélène; Gao, Junjun; Golling, Sabrina; Lamerz, Jens; Le Pogam, Sophie; Tzouros, Manuel; Sankabathula, Sailaja; Gruenbaum, Lore; Nájera, Isabel; Langen, Hanno; Klumpp, Klaus; Augustin, Angélique

    2014-11-01

    Mapping protein-protein interactions is essential to fully characterize the biological function of a protein and improve our understanding of diseases. Affinity purification coupled to mass spectrometry (AP-MS) using selective antibodies against a target protein has been commonly applied to study protein complexes. However, one major limitation is a lack of specificity as a substantial part of the proposed binders is due to nonspecific interactions. Here, we describe an innovative immuno-competitive capture mass spectrometry (ICC-MS) method to allow systematic investigation of protein-protein interactions. ICC-MS markedly increases the specificity of classical immunoprecipitation (IP) by introducing a competition step between free and capturing antibody prior to IP. Instead of comparing only one experimental sample with a control, the methodology generates a 12-concentration antibody competition profile. Label-free quantitation followed by a robust statistical analysis of the data is then used to extract the cellular interactome of a protein of interest and to filter out background proteins. We applied this new approach to specifically map the interactome of hepatitis C virus (HCV) nonstructural protein 5A (NS5A) in a cellular HCV replication system and uncovered eight new NS5A-interacting protein candidates along with two previously validated binding partners. Follow-up biological validation experiments revealed that large tumor suppressor homolog 1 and 2 (LATS1 and LATS2, respectively), two closely related human protein kinases, are novel host kinases responsible for NS5A phosphorylation at a highly conserved position required for optimal HCV genome replication. These results are the first illustration of the value of ICC-MS for the analysis of endogenous protein complexes to identify biologically relevant protein-protein interactions with high specificity.

  10. 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

  11. 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.

  12. 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

  13. 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

  14. 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.

  15. 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

  16. 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.

  17. 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...

  18. 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...

  19. 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...

  20. 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.

  1. Proton transfer reaction-mass spectrometry: online and rapid determination of volatile organic compounds of microbial origin.

    Science.gov (United States)

    Romano, Andrea; Capozzi, Vittorio; Spano, Giuseppe; Biasioli, Franco

    2015-05-01

    Analytical tools for the identification and quantification of volatile organic compounds (VOCs) produced by microbial cultures have countless applications in an industrial and research context which are still not fully exploited. The various techniques for VOC analysis generally arise from the application of different scientific and technological philosophies, favoring either sample throughput or chemical information. Proton transfer reaction-mass spectrometry (PTR-MS) represents a valid compromise between the two aforementioned approaches, providing rapid and direct measurements along with highly informative analytical output. The present paper reviews the main applications of PTR-MS in the microbiological field, comprising food, environmental, and medical applications.

  2. CO{sub 2} capture using fly ash-derived activated carbons impregnated with low molecular mass amines

    Energy Technology Data Exchange (ETDEWEB)

    Smith, K.M.; Arenillas, A.; Drage, T.C.; Snape, C.E. [University of Nottingham, Nottingham (United Kingdom). Nottingham Fuel and Energy Centre

    2005-07-01

    Two different approaches to develop high capacity CO{sub 2} sorbents are presented. Firstly, the modification of the surface chemistry of low cost carbons by impregnation with a basic nitrogen-containing polymer (i.e.polyethylenimine) is described. Relatively low molecular mass (MM) amines, namely diethanolamine (DEA, MM 105) and tetraethylenepentaamineacrylonitrile (TEPAN, MM 311) are used to produce high capacity CO{sub 2} sorbents from activated carbons derived from unburned carbon in fly ash, which have low mesoporosities. The CO{sub 2} adsorption capacity and thermal stability of the prepared sorbents was measured as a function of temperature in a thermogravimetric analyser. The results indicate that TEPAN is more effective than DEA; at a temperature of 75{sup o}C, fly ash-derived activated carbons loaded with TEPAN achieved CO{sub 2} adsorption capacities in excess of 5 wt%, which compares fabvourably with the CO{sub 2} absorption capacity of 6.5 wt% achieved with a mesoporous silica loaded with TEPAN, and outperforms fly ash-derived activated carbons loaded with PEI. TEPAN has also been shown to have a higher thermal stability than DEA. The second approach involves the development of high nitrogen content carbon matrix adsorbents by carbonisation and subsequent thermal or chemical activation of a range of materials (polyacrylonitrile, glucose-amine mixtures, melamine and urea/melamine-formaldehyde resins). The results show that although the amount of nitrogen incorporated to the final adsorbent is important, the N-functionality seems to be more relevant for increasing CO{sub 2} uptake. However, the adsorbent obtained from carbazole-sugar co-pyrolysis, despite the lower amount of N incorporated, shows high CO{sub 2} uptake, up to 9 wt%, probably because the presence of more basic functionalities as determined by XPS analysis. 9 refs., 2 figs.

  3. 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.

  4. 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

  5. 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.

  6. 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

  7. Chapter 3. Determination of semivolatile organic compounds and polycyclic aromatic hydrocarbons in solids by gas chromatography/mass spectrometry

    Science.gov (United States)

    Zaugg, Steven D.; Burkhardt, Mark R.; Burbank, Teresa L.; Olson, Mary C.; Iverson, Jana L.; Schroeder, Michael P.

    2006-01-01

    A method for the determination of 38 polycyclic aromatic hydrocarbons (PAHs) and semivolatile organic compounds in solid samples is described. Samples are extracted using a pressurized solvent extraction system. The compounds of interest are extracted from the solid sample twice at 13,800 kilopascals; first at 120 degrees Celsius using a water/isopropyl alcohol mixture (50:50, volume-to-volume ratio), and then the sample is extracted at 200 degrees Celsius using a water/isopropyl alcohol mixture (80:20, volume-to-volume ratio). The compounds are isolated using disposable solid-phase extraction (SPE) cartridges containing divinylbenzene-vinylpyrrolidone copolymer resin. The cartridges are dried with nitrogen gas, and then sorbed compounds are eluted from the SPE material using a dichloromethane/diethyl ether mixture (80:20, volume-to-volume ratio) and passed through a sodium sulfate/Florisil SPE cartridge to remove residual water and to further clean up the extract. The concentrated extract is solvent exchanged into ethyl acetate and the solvent volume reduced to 0.5 milliliter. Internal standard compounds are added prior to analysis by capillary-column gas chromatography/mass spectrometry. Comparisons of PAH data for 28 sediment samples extracted by Soxhlet and the accelerated solvent extraction (ASE) method described in this report produced similar results. Extraction of PAH compounds from standard reference material using this method also compared favorably with Soxhlet extraction. The recoveries of PAHs less than molecular weight 202 (pyrene or fluoranthene) are higher by up to 20 percent using this ASE method, whereas the recoveries of PAHs greater than or equal to molecular weight 202 are equivalent. This ASE method of sample extraction of solids has advantages over conventional Soxhlet extraction by increasing automation of the extraction process, reducing extraction time, and using less solvent. Extract cleanup also is greatly simplified because SPE replaces

  8. 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

  9. 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

  10. Applications of information theory and pattern recognition to gas chromatography-mass spectrometric analysis of toxic organic compounds in ambient air

    Energy Technology Data Exchange (ETDEWEB)

    Scott, D.R.

    1986-05-01

    The number of information channels contained in the gas-chromatographic, mass-spectrometric, and combined gas chromatography-mass spectrometric analysis of 78 toxic organic compounds was determined. The toxic compounds are those routinely monitored in ambient air samples using Tenax collection and gas chromatography-mass spectrometric analysis. The Shannon information content of the binary encoded and full-intensity mass spectra, of the gas-chromatographic retention times, and of the combined gas chromatographic-mass spectrometric spectra of the 78 compounds was calculated. The maximum binary information contents of the 35 channel gas chromatographic, 17 key channel mass spectral, and the 595 channel gas chromatographic-mass spectral methods were 6.4, 15.4, and < 21.8 bits, respectively. The 17 masses with the highest binary information content with regard to the 78 compounds were used with SIMCA pattern recognition to determine four classes among the 78 compounds. These included aromatics without chlorine substitution, chloroaromatics, bromoalkanes and alkenes, and chloroalkanes and alkenes.

  11. 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.

  12. 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.

  13. 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 ...

  14. 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. ...

  15. 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...

  16. 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

  17. Supercritical fluid chromatography coupled with in-source atmospheric pressure ionization hydrogen/deuterium exchange mass spectrometry for compound speciation.

    Science.gov (United States)

    Cho, Yunju; Choi, Man-Ho; Kim, Byungjoo; Kim, Sunghwan

    2016-04-29

    An experimental setup for the speciation of compounds by hydrogen/deuterium exchange (HDX) with atmospheric pressure ionization while performing chromatographic separation is presented. The proposed experimental setup combines the high performance supercritical fluid chromatography (SFC) system that can be readily used as an inlet for mass spectrometry (MS) and atmospheric pressure photo ionization (APPI) or atmospheric pressure chemical ionization (APCI) HDX. This combination overcomes the limitation of an approach using conventional liquid chromatography (LC) by minimizing the amount of deuterium solvents used for separation. In the SFC separation, supercritical CO2 was used as a major component of the mobile phase, and methanol was used as a minor co-solvent. By using deuterated methanol (CH3OD), AP HDX was achieved during SFC separation. To prove the concept, thirty one nitrogen- and/or oxygen-containing standard compounds were analyzed by SFC-AP HDX MS. The compounds were successfully speciated from the obtained SFC-MS spectra. The exchange ions were observed with as low as 1% of CH3OD in the mobile phase, and separation could be performed within approximately 20min using approximately 0.24 mL of CH3OD. The results showed that SFC separation and APPI/APCI HDX could be successfully performed using the suggested method.

  18. 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.

  19. Speciation of butyltin compounds in marine sediments with headspace solid phase microextraction and gas chromatography - mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Cardellicchio, N.; Giandomenico, S.; Decataldo, A.; Di Leo, A. [CNR - Istituto Sperimentale Talassografico, Taranto (Italy)

    2001-03-01

    A method for the determination of organotin compounds (monobutyl = MBT, dibutyl = DBT, and tributyltin = TBT) in marine sediments by headspace Solid Phase Microextraction (SPME) has been developed. The analytical procedure involved 1) extraction of TBT, DBT and MBT from sediments with HCl and methanol mixture, 2) in situ derivatization with sodium tetraethylborate and 3) headspace SPME extraction using a fiber coated with poly(dimethylsiloxane). The derivatized organotin compounds were desorbed into the splitless injector and simultaneously analyzed by gas chromatography - mass spectrometry.The analytical method was optimized with respect to derivatization reaction and extraction conditions. The detection limits obtained for MBT, DBT and TBT ranged from 730 to 969 pg/g as Sn dry weight. Linear calibration curves were obtained for all analytes in the range of 30-1000 ng/L as Sn. Analysis of a standard reference sediment (CRM 462) demonstrates the suitability of this method for the determination of butyltin compounds in marine sediments. The application to the determination of TBT, DBT and MBT in a coastal marine sediment is shown. (orig.)

  20. Speciation of butyltin compounds in marine sediments with headspace solid phase microextraction and gas chromatography mass spectrometry.

    Science.gov (United States)

    Cardellicchio, N; Giandomenico, S; Decataldo, A; Di Leo, A

    2001-03-01

    A method for the determination of organotin compounds (monobutyl = MBT, dibutyl = DBT, and tributyltin = TBT) in marine sediments by headspace Solid Phase Microextraction (SPME) has been developed. The analytical procedure involved 1) extraction of TBT, DBT and MBT from sediments with HCl and methanol mixture, 2) in situ derivatization with sodium tetraethylborate and 3) headspace SPME extraction using a fiber coated with poly(dimethylsiloxane). The derivatized organotin compounds were desorbed into the splitless injector and simultaneously analyzed by gas chromatography - mass spectrometry. The analytical method was optimized with respect to derivatization reaction and extraction conditions. The detection limits obtained for MBT, DBT and TBT ranged from 730 to 969 pg/g as Sn dry weight. Linear calibration curves were obtained for all analytes in the range of 30-1000 ng/L as Sn. Analysis of a standard reference sediment (CRM 462) demonstrates the suitability of this method for the determination of butyltin compounds in marine sediments. The application to the determination of TBT, DBT and MBT in a coastal marine sediment is shown. PMID:11336336

  1. Ambient Observations of Organic Nitrogen Compounds in Submicrometer Aerosols in New York Using High Resolution Aerosol Mass Spectrometry

    Science.gov (United States)

    Zhou, S.; Ge, X.; Xu, J.; Sun, Y.; Zhang, Q.

    2015-12-01

    Organic nitrogen (ON) compounds, which include amines, nitriles, organic nitrates, amides, and N-containing aromatic heterocycles, are an important class of compounds ubiquitously detected in atmospheric particles and fog and cloud droplets. Previous studies indicate that these compounds can make up a significant fraction (20-80%) of the total nitrogen (N) content in atmospheric condensed phases and play important roles in new particle formation and growth and affecting the optical and hygroscopicity of aerosols. In this study, we report the observation of ON compounds in submicrometer particles (PM1) at two locations in New York based on measurements using Aerodyne high-resolution time-of-flight mass spectrometer (HR-ToF-AMS). One study was conducted as part of the US Department of Energy funded Aerosol Lifecyle - Intensive Operation Period (ALC-IOP) campaign at Brookhaven National Lab (BNL, 40.871˚N, 72.89˚W) in summer, 2011 and the other was conducted at the Queen's College (QC) in New York City (NYC) in summer, 2009. We observed a notable amount of N-containing organic fragment ions, CxHyNp+ and CxHyOzNp+, in the AMS spectra of organic aerosols at both locations and found that they were mainly associated with amino functional groups. Compared with results from lab experiments, the C3H8N+ at m/z = 58 was primarily attributed to trimethylamine. In addition, a significant amount of organonitrates was observed at BNL. Positive matrix factorization (PMF) analysis of the high resolution mass spectra (HRMS) of organic aerosols identified a unique nitrogen-enriched OA (NOA) factor with elevated nitrogen-to-carbon (N/C) at both BNL and QC. Analysis of the size distributions, volatility profiles, and correlations with external tracer indicates that acid-base reactions of amino compounds with sulfate and acidic gas were mainly responsible for the formation of amine salts. Photochemical production was also observed to play a role in the formation of NOA. Bivariate polar

  2. 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

  3. 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)

  4. Nigriventrine: a low molecular mass neuroactive compound from the venom of the spider Phoneutria nigriventer.

    Science.gov (United States)

    Gomes, Paulo C; de Souza, Bibiana M; Dias, Nathalia B; Cesar-Tognoli, Lilian M M; Silva-Filho, Luiz C; Tormena, Cláudio F; Rittner, Roberto; Richardson, Michael; Cordeiro, Marta N; Palma, Mario S

    2011-02-01

    Nigriventrine was isolated from the "armed" spider Phoneutria nigriventer, in which it constitutes about 0.4% of the total venom content. Its structure was determined to be [1,1'-(1-hydroxyhydrazine-1,2-diyl)bis(oxy)bis(4-hydroxy-2,6-dioxopiperidine-4 carboxylic acid)] by NMR, HR-ES/IMS and MS/MS methods. The intracerebroventricular application of nigriventrine in rat brain, followed by the detection of c-Fos protein expression, indicated that the compound was neuroactive in the motor cortex, sensory cortex, piriform cortex, median preoptic nucleus, dorsal endopiriform nucleus, lateral septal nucleus and hippocampus of rat brain. Nigriventrine causes convulsions in rats, even when peripherally applied.

  5. 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.

  6. 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.

  7. 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.

  8. 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)

  9. Optimization and application of atmospheric pressure chemical and photoionization hydrogen-deuterium exchange mass spectrometry for speciation of oxygen-containing compounds.

    Science.gov (United States)

    Acter, Thamina; Kim, Donghwi; Ahmed, Arif; Jin, Jang Mi; Yim, Un Hyuk; Shim, Won Joon; Kim, Young Hwan; Kim, Sunghwan

    2016-05-01

    This paper presents a detailed investigation of the feasibility of optimized positive and negative atmospheric pressure chemical ionization (APCI) mass spectrometry (MS) and atmospheric pressure photoionization (APPI) MS coupled to hydrogen-deuterium exchange (HDX) for structural assignment of diverse oxygen-containing compounds. The important parameters for optimization of HDX MS were characterized. The optimized techniques employed in the positive and negative modes showed satisfactory HDX product ions for the model compounds when dichloromethane and toluene were employed as a co-solvent in APCI- and APPI-HDX, respectively. The evaluation of the mass spectra obtained from 38 oxygen-containing compounds demonstrated that the extent of the HDX of the ions was structure-dependent. The combination of information provided by different ionization techniques could be used for better speciation of oxygen-containing compounds. For example, (+) APPI-HDX is sensitive to compounds with alcohol, ketone, or aldehyde substituents, while (-) APPI-HDX is sensitive to compounds with carboxylic functional groups. In addition, the compounds with alcohol can be distinguished from other compounds by the presence of exchanged peaks. The combined information was applied to study chemical compositions of degraded oils. The HDX pattern, double bond equivalent (DBE) distribution, and previously reported oxidation products were combined to predict structures of the compounds produced from oxidation of oil. Overall, this study shows that APCI- and APPI-HDX MS are useful experimental techniques that can be applied for the structural analysis of oxygen-containing compounds.

  10. [Coupling of gas chromatography with single photon ionization time-of-flight mass spectrometry and its application to characterization of compounds in diesel].

    Science.gov (United States)

    Xie, Yuanyuan; Hua, Lei; Chen, Ping; Hou, Keyong; Jiang, Jichun; Wang, Yan; Li, Haiyang

    2015-02-01

    A novel analytical method coupling gas chromatography (GC) with single photon ionization time-of-flight mass spectrometry (SPI-TOF MS) has been developed. First of all, a double-wall-tube transfer line was built to combine GC with SPI-TOF MS, which realized seamless connection between GC and SPI ion source. Based on this, standard n-pentadecane and benzene/toluene/xylene standard gas mixtures were used to study important voltage parameters of the ion source. After the optimization of the ion source voltages, pure molecular ion peaks of the analytes were obtained in the mass spectra and qualitative analysis of different kinds of organic compounds were eventually realized rapidly and accurately. At last, GC/SPI-TOF MS was applied to the characterization of volatile and semvolatile organic compounds in diesel and two-dimensional spectra of GC×SPI-TOF MS were obtained. Without complicated spectra interpretation and data processing, volatile and semi-volatile organic compounds in diesel have been classified qualitatively by ion mass-to-charge ratio (m/z) in SPI mass spectra, including aliphatic compounds, aromatic compounds and nitrogen-containing compounds with low concentration such as benzopyrroles. Isomeric compounds in diesel were separated and identified by retention times of chromatographic peaks. The results indicate that the proposed analytical method of GC/SPI-TOF MS is suitable for the characterization of complicated samples such as diesel and environmental pollutants with easy operation and high efficiency.

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

    CERN Document Server

    Valdre', S; Casini, G; Pasquali, G; Piantelli, S; Carboni, S; Cinausero, M; Gramegna, F; Marchi, T; Baiocco, G; Bardelli, L; Benzoni, G; Bini, M; Blasi, N; Bracco, A; Brambilla, S; Bruno, M; Camera, F; Corsi, A; Crespi, F; Agostino, M D; Degerlier, M; Kravchuk, V L; Leoni, S; Million, B; Montanari, D; Morelli, L; Nannini, A; Nicolini, R; Poggi, G; Vannini, G; Wieland, O; Bednarczyk, P; Ciemała, M; Dudek, J; Fornal, B; Kmiecik, M; Maj, A; Matejska-Minda, M; Mazurek, K; Meczynski, W; Myalski, S; Styczen, J; Zieblinski, M

    2013-01-01

    The 48Ti on 40Ca reactions have been studied at 300 and 600 MeV focusing on the fusion-evaporation (FE) and fusion-fission (FF) exit channels. Energy spectra and multiplicities of the emitted light charged particles have been compared to Monte Carlo simulations based on the statistical model. Indeed, in this mass region (A about 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 preequilibrium emissions from 300 to 600 MeV bombarding energy.

  12. Growth of Candida albicans in human saliva is supported by low-molecular-mass compounds.

    Science.gov (United States)

    Valentijn-Benz, Marianne; Nazmi, Kamran; Brand, Henk S; van't Hof, Wim; Veerman, Enno C I

    2015-12-01

    Saliva plays a key role in the maintenance of a stable oral microflora. It contains antimicrobial compounds but also functions as a substrate for growth of bacteria under conditions of low external nutrient supply. Besides bacteria, yeasts, in particular Candida albicans, commonly inhabit the oral cavity. Under immunocompromised conditions, instantaneous outgrowth of this yeast occurs in oral carriers of C. albicans, suggesting that this yeast is able to survive in the oral cavity with saliva as sole source of growth substrate. The aim of the present study was to identify the salivary constituents that are used by C. albicans for growth and survival in saliva. In addition, we have explored the effect of growth in saliva on the susceptibility of C. albicans to histatin 5, a salivary antifungal peptide. It was found that C. albicans was able to grow in human saliva without addition of glucose, and in the stationary phase could survive for more than 400 h. Candida albicans grown in saliva was more than 10 times less susceptible for salivary histatin 5 than C. albicans cultured in Sabouraud medium.

  13. Selected Ion Flow-Drift Tube Mass Spectrometry: Quantification of Volatile Compounds in Air and Breath.

    Science.gov (United States)

    Spesyvyi, Anatolii; Smith, David; Španěl, Patrik

    2015-12-15

    A selected ion flow-drift tube mass spectrometric analytical technique, SIFDT-MS, is described that extends the established selected ion flow tube mass spectrometry, SIFT-MS, by the inclusion of a static but variable E-field along the axis of the flow tube reactor in which the analytical ion-molecule chemistry occurs. The ion axial speed is increased in proportion to the reduced field strength E/N (N is the carrier gas number density), and the residence/reaction time, t, which is measured by Hadamard transform multiplexing, is correspondingly reduced. To ensure a proper understanding of the physics and ion chemistry underlying SIFDT-MS, ion diffusive loss to the walls of the flow-drift tube and the mobility of injected H3O(+) ions have been studied as a function of E/N. It is seen that the derived diffusion coefficient and mobility of H3O(+) ions are consistent with those previously reported. The rate coefficient has been determined at elevated E/N for the association reaction of the H3O(+) reagent ions with H2O molecules, which is the first step in the production of H3O(+)(H2O)1,2,3 reagent hydrate ions. The production of hydrated analyte ion was also experimentally investigated. The analytical performance of SIFDT-MS is demonstrated by the quantification of acetone and isoprene in exhaled breath. Finally, the essential features of SIFDT-MS and SIFT-MS are compared, notably pointing out that a much lower speed of the flow-drive pump is required for SIFDT-MS, which facilitates the development of smaller cost-effective analytical instruments for real time breath and fluid headspace analyses.

  14. 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.

  15. 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....

  16. 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.

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

    Science.gov (United States)

    Valdré, S.; Barlini, S.; Casini, G.; Pasquali, G.; Piantelli, S.; Carboni, S.; Cinausero, M.; Gramegna, F.; Marchi, T.; Baiocco, G.; Bardelli, L.; Benzoni, G.; Bini, M.; Blasi, N.; Bracco, A.; Brambilla, S.; Bruno, M.; Camera, F.; Corsi, A.; Crespi, F.; D'Agostino, M.; Degerlier, M.; Kravchuk, V. L.; Leoni, S.; Million, B.; Montanari, D.; Morelli, L.; Nannini, A.; Nicolini, R.; Poggi, G.; Vannini, G.; Wieland, O.; Bednarczyk, P.; Ciemała, M.; Dudek, J.; Fornal, B.; Kmiecik, M.; Maj, A.; Matejska-Minda, M.; Mazurek, K.; Męczyński, W. M.; Myalski, S.; Styczeń, J.; Ziębliński, M.

    2014-03-01

    The 48Ti on 40Ca reactions have been studied at 300 and 600 MeV focusing on the fusion-evaporation (FE) and fusion-fission (FF) exit channels. Energy spectra and multiplicities of the emitted light charged particles have been compared to Monte Carlo simulations based on the statistical model. 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. 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.

  19. 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

  20. 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

  1. 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.

  2. 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...

  3. 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.

  4. 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

  5. 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.

  6. 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

  7. 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 ...

  8. [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

  9. 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

  10. Argon direct analysis in real time mass spectrometry in conjunction with makeup solvents: a method for analysis of labile compounds.

    Science.gov (United States)

    Yang, Hongmei; Wan, Debin; Song, Fengrui; Liu, Zhiqiang; Liu, Shuying

    2013-02-01

    Helium direct analysis in real time (He-DART) mass spectrometry (MS) analysis of labile compounds usually tends to be challenging because of the occurrence of prominent fragmentation, which obscures the assigning of an ion to an independent species or merely a fragment in a mixture. In the present work, argon DART (Ar-DART) MS in conjunction with makeup solvents has been demonstrated to analyze a variety of labile compounds including nucleosides, alkaloids, glucose, and other small molecules. The results presented here confirm that Ar-DART can generate significantly less energetic ions than conventional He-DART and is able to produce the intact molecular ions with little or no fragmentation in both positive and negative ion modes. Adding a makeup solvent (absolute ethyl alcohol, methanol, fluorobenzene, or acetone) to the argon gas stream at the exit of the DART ion source can result in 1-2 orders of magnitude increase in detection signals. The sensitivity attainable by Ar-DART was found to be comparable to that by He-DART. The investigation of influence of solvents improves our understanding of the fundamental desorption and ionization processes in DART. The practical application of this rapid and high throughput method is demonstrated by the successful analysis of a natural product (Crude Kusnezoff Monkshood) extract, demonstrating the great potential in mixture research.

  11. Diagnostic determination of melamine and related compounds in kidney tissue by liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Filigenzi, Michael S; Puschner, Birgit; Aston, Linda S; Poppenga, Robert H

    2008-09-10

    In 2007, it was determined that melamine, ammeline, ammelide, and cyanuric acid (abbreviated as MARC for melamine and related contaminants) had been added to wheat gluten and rice protein that were subsequently incorporated into pet food. The consumption of food tainted by MARC compounds was implicated in numerous instances of renal failure in cats and dogs. A method for the analysis of MARC compounds in kidney tissue using high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS) has been developed. MARC analytes were extracted by homogenization of kidney tissue in 50/40/10 acetonitrile/water/diethylamine. The homogenate was centrifuged, and an aliquot of supernatant was diluted with acetonitrile, concentrated, and fortified with a stable isotope-labeled analogue of melamine. Analytes were detected using atmospheric pressure chemical ionization and multiple reaction monitoring. Quantitation of positive samples was performed using the internal standard method and five-point calibration curves ranging between 50 and 1000 ng/mL of each analyte. The method was validated by analysis of replicate kidney tissue samples fortified with the individual analytes and by analysis of kidney samples fortified with melamine cyanurate powder at two different concentrations. This method was successfully used for routine postmortem diagnosis of melamine toxicosis in animals. Melamine was also detected by this method in paraffin-embedded tissue from animals suspected to have died of melamine toxicosis. PMID:18652475

  12. Sensitive Detection of Aromatic Hydrophobic Compounds in Water and Perfluorooctane Sulfonate in Human Serum by Surface-Assisted Laser Desorption/Ionization Mass Spectrometry (SALDI-MS) with Amine Functionalized Graphene-Coated Cobalt Nanoparticles.

    Science.gov (United States)

    Nakai, Keisuke; Kawasaki, Hideya; Yamamoto, Atsushi; Arakawa, Ryuichi; Grass, Robert N; Stark, Wendelin J

    2014-01-01

    In this article, we describe the application of surface-assisted laser desorption/ionization mass spectrometry (SALDI-MS) with the use of amine functionalized graphene-coated cobalt nanoparticles (CoC-NH2 nanoparticles) to analyse aromatic hydrophobic compounds that are known environmental contaminants, including polycyclic aromatic hydrocarbons (PAHs) and pentachlorophenol (PCP). Our results demonstrated that SALDI-MS can detect PCP, anthracene, and pyrene in water. In particular, the CoC-NH2 nanoparticles proved to be an efficient means of capturing PCP in water because of the high adsorption capacity of the nanoparticles for PCP, which resulted in a detectability of 100 ppt. Furthermore, the CoC-NH2 nanoparticles also functioned as an adsorbent for solid-phase extraction of perfluorooctane sulfonate (PFOS) from human serum, displaying good performance with a detectability of 10 ppb by SALDI-MS.

  13. 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.

  14. Insights into the Binding Sites of Organometallic Ruthenium Anticancer Compounds on Peptides Using Ultra-High Resolution Mass Spectrometry

    Science.gov (United States)

    Wills, Rebecca H.; Habtemariam, Abraha; Lopez-Clavijo, Andrea F.; Barrow, Mark P.; Sadler, Peter J.; O'Connor, Peter B.

    2014-04-01

    The binding sites of two ruthenium(II) organometallic complexes of the form [(η6-arene)Ru( N, N)Cl]+, where arene/ N, N = biphenyl (bip)/bipyridine (bipy) for complex AH076, and biphenyl (bip)/ o-phenylenediamine ( o-pda) for complex AH078, on the peptides angiotensin and bombesin have been investigated using Fourier transform ion cyclotron resonance (FTICR) mass spectrometry. Fragmentation was performed using collisionally activated dissociation (CAD), with, in some cases, additional data being provided by electron capture dissociation (ECD). The primary binding sites were identified as methionine and histidine, with further coordination to phenylalanine, potentially through a π-stacking interaction, which has been observed here for the first time. This initial peptide study was expanded to investigate protein binding through reaction with insulin, on which the binding sites proposed are histidine, glutamic acid, and tyrosine. Further reaction of the ruthenium complexes with the oxidized B chain of insulin, in which two cysteine residues are oxidized to cysteine sulfonic acid (Cys-SO3H), and glutathione, which had been oxidized with hydrogen peroxide to convert the cysteine to cysteine sulfonic acid, provided further support for histidine and glutamic acid binding, respectively.

  15. 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

  16. 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

  17. Unexpected tolerance of glycosylation by UDP-GalNAc:polypeptide alpha-N-acetylgalactosaminyltransferase revealed by electron capture dissociation mass spectrometry: carbohydrate as potential protective groups.

    Science.gov (United States)

    Yoshimura, Yayoi; Matsushita, Takahiko; Fujitani, Naoki; Takegawa, Yasuhiro; Fujihira, Haruhiko; Naruchi, Kentarou; Gao, Xiao-Dong; Manri, Naomi; Sakamoto, Takeshi; Kato, Kentaro; Hinou, Hiroshi; Nishimura, Shin-Ichiro

    2010-07-20

    UDP-GalNAc:polypeptide alpha-N-acetylgalactosaminyltransferases (ppGalNAcTs, EC 2.4.1.41), a family of key enzymes that initiate posttranslational modification with O-glycans in mucin synthesis by introduction of alpha-GalNAc residues, are structurally composed of a catalytic domain and a lectin domain. It has been known that multiple Ser/Thr residues are assigned in common mucin glycoproteins as potential O-glycosylation sites and more than 20 distinct isoforms of this enzyme family contribute to produce densely O-glycosylated mucin glycoproteins. However, it seems that the functional role of the lectin domain of ppGalNAcTs remains unclear. We considered that electron capture dissociation mass spectrometry (ECD-MS), a promising method for highly selective fragmentation at peptide linkages of glycopeptides to generate unique c and z series of ions, should allow for precise structural characterization to uncover the mechanism in O-glycosylation of mucin peptides by ppGalNAcTs. In the present study, it was demonstrated that a system composed of an electrospray source, a linear RFQ ion trap that isolates precursor ions, the ECD device, and a TOF mass spectrometer is a nice tool to identify the preferential O-glycosylation sites without any decomposition of the carbohydrate moiety. It should be noted that electrons used for ECD are accelerated within a range from 1.75 to 9.75 eV depending on the structures of glycopeptides of interest. We revealed for the first time that additional installation of a alpha-GalNAc residue at potential glycosylation sites by ppGalNAcT2 proceeds smoothly in various unnatural glycopeptides having alpha-Man, alpha-Fuc, and beta-Gal residues as well as alpha-GalNAc residues. The results may suggest that ppGalNAcT2 did not differentiate totally presubstituted sugar residues in terms of configuration of functional groups, d-, l-configuration, and even alpha-, beta-stereochemistry at an anomeric carbon atom when relatively short synthetic

  18. 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,

  19. 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. L. Sun

    2010-05-01

    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 Chromatography system (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, m/z 306 (C

  20. 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

  1. Tentative identification of polar and mid-polar compounds in extracts from wine lees by liquid chromatography-tandem mass spectrometry in high-resolution mode.

    Science.gov (United States)

    Delgado de la Torre, M P; Priego-Capote, F; Luque de Castro, M D

    2015-06-01

    Sustainable agriculture has a pending goal in the revalorization of agrofood residues. Wine lees are an abundant residue in the oenological industry. This residue, so far, has been used to obtain tartaric acid or pigments but not for being qualitatively characterized as a source of polar and mid-polar compounds such as flavonoids, phenols and essential amino acids. Lees extracts from 11 Spanish wineries have been analyzed by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) in high resolution mode. The high-resolution power of LC-MS/MS has led to the tentative identification of the most representative compounds present in wine lees, comprising primary amino acids, anthocyans, flavanols, flavonols, flavones and non-flavonoid phenolic compounds, among others. Attending to the profile and content of polar and mid-polar compounds in wine lees, this study underlines the potential of wine lees as an exploitable source to isolate interesting compounds.

  2. 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.

  3. 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

    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......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...... + H - H2O](+), whereas the reverse situation characterized the sn-3 species. Furthermore, corresponding sn-2 and sn-3 species were separated by the chromatographic system. However, loss of water was promoted as fatty acid unsaturation was raised, which may complicate interpretation of the mass spectra...

  4. 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

  5. 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.

  6. Determination of endocrine-disrupting compounds in drinking waters by fast liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Magi, Emanuele; Scapolla, Carlo; Di Carro, Marina; Liscio, Camilla

    2010-09-01

    Growing attention has been recently paid to safety of food and drinking water, making necessary the adoption of policies for water sources protection and the development of sensitive and rapid analytical methods to identify micropollutants. Endocrine-disrupting compounds (EDCs) have emerged as a major issue as they alter the functioning of the endocrine system. Since ingestion of EDCs via food is considered the major exposure route, there is a growing interest in understanding EDC fate during drinking water treatment and in monitoring potential contamination of surface waters and groundwaters. In this work, a fast liquid chromatography-electrospray ionization-tandem mass spectrometry method was developed for the determination of 4-n-nonylphenol (NP), bisphenol A (BPA), estrone (E1), 17β-estradiol (E2) and 17α-ethinylestradiol (EE2) in drinking waters. In the literature analytical articles seldom provide details regarding fragmentation pathways. In this paper spectra of the five EDCs in negative ESI were interpreted with the support of accurate mass spectra acquired by a quadrupole time-of-flight instrument; fragmentation pathways were also proposed. The chromatographic separation of EDCs was optimized on a Pinnacle DB Biphenylic column with a water-acetonitrile gradient. Quantitative analysis was performed in multiple reaction monitoring (MRM) mode using bisphenol A-d(16) (BPA-d(16)) as internal standard; calibration curves showed good correlation coefficients (0.9989-0.9997). All figures of merit of the method were satisfactory; limits of detection were in the range 0.2-0.4 ng/ml. The method was applied to the determination of the analytes in waters sampled by polar organic chemical integrative samplers in a drinking water treatment plant. Rather low concentration of BPA, NP and E1 were measured in the inlet, while none of the considered EDCs was detected in the outlet.

  7. Black phosphorus-assisted laser desorption ionization mass spectrometry for the determination of low-molecular-weight compounds in biofluids.

    Science.gov (United States)

    He, Xiao-Mei; Ding, Jun; Yu, Lei; Hussain, Dilshad; Feng, Yu-Qi

    2016-09-01

    Quantitative analysis of small molecules by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) has been a challenging task due to matrix-derived interferences in low m/z region and poor reproducibility of MS signal response. In this study, we developed an approach by applying black phosphorus (BP) as a matrix-assisted laser desorption ionization (MALDI) matrix for the quantitative analysis of small molecules for the first time. Black phosphorus-assisted laser desorption/ionization mass spectrometry (BP/ALDI-MS) showed clear background and exhibited superior detection sensitivity toward quaternary ammonium compounds compared to carbon-based materials. By combining stable isotope labeling (SIL) strategy with BP/ALDI-MS (SIL-BP/ALDI-MS), a variety of analytes labeled with quaternary ammonium group were sensitively detected. Moreover, the isotope-labeled forms of analytes also served as internal standards, which broadened the analyte coverage of BP/ALDI-MS and improved the reproducibility of MS signals. Based on these advantages, a reliable method for quantitative analysis of aldehydes from complex biological samples (saliva, urine, and serum) was successfully established. Good linearities were obtained for five aldehydes in the range of 0.1-20.0 μM with correlation coefficients (R (2)) larger than 0.9928. The LODs were found to be 20 to 100 nM. Reproducibility of the method was obtained with intra-day and inter-day relative standard deviations (RSDs) less than 10.4 %, and the recoveries in saliva samples ranged from 91.4 to 117.1 %. Taken together, the proposed SIL-BP/ALDI-MS strategy has proved to be a reliable tool for quantitative analysis of aldehydes from complex samples. Graphical Abstract An approach for the determination of small molecules was developed by using black phosphorus (BP) as a matrix-assisted laser desorption ionization (MALDI) matrix.

  8. 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

  9. 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.

  10. 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.

  11. 2-Hydrazinoquinoline: a reactive matrix for matrix-assisted laser desorption/ionization mass spectrometry to detect gaseous carbonyl compounds.

    Science.gov (United States)

    Shigeri, Yasushi; Kamimura, Takuya; Ando, Masanori; Uegaki, Koichi; Sato, Hiroaki; Tani, Fumito; Arakawa, Ryuichi; Kinumi, Tomoya

    2016-01-01

    The sensitivity, range of applications, and reaction mechanism of 2-hydrazinoquinoline as a reactive matrix for matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) were examined. Using a reaction chamber (125L) equipped with a stirring fan and a window for moving the MALDI-MS plate and volatile samples in and out, the sensitivities of 2-hydrazinoquinoline to gaseous aldehydes (formaldehyde, acetaldehyde, propionaldehyde, and n-butyraldehyde) and ketones (acetone, methyl ethyl ketone, and methyl isobutyl ketone) were determined to be at least parts per million (ppm) levels. On the other hand, carboxylic acids (formic acid, acetic acid, propionic acid, and butyric acid) and esters (ethyl acetate, pentyl acetate, isoamyl acetate, and methyl salicylate) could not be detected by 2-hydrazinoquinoline in MALDI-MS. In addition to 2,4-dinitrophenylhydrazine, a common derivatization reagent for analyzing carbonyl compounds quantitatively in gas chromatography and liquid chromatography, the dissolution of 2-hydrazinoquinoline in an acidic solution, such as trifluoroacetic acid, was essential for its function as a reactive matrix for MALDI- MS. PMID:27419901

  12. 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

  13. 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.)

  14. 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.)

  15. 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

  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

    Three water-soluble aliphatic arsenicals, dimethylarsinoyl acetate (DMAA), dimethylarsinoyl ethanol (DMAE), and dimethylarsinoyl propionate (DMAP), were identified in marine biological samples. Sample extracts in methanol/water (1 + 1) were analysed by cation-exchange high-performance liquid...... 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...

  17. 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 ...

  18. 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...

  19. Sequential ultrasonic extraction of a Chinese coal and characterization of nitrogen-containing compounds in the extracts using high-performance liquid chromatography with mass spectrometry.

    Science.gov (United States)

    Xia, Jun-Liu; Fan, Xing; You, Chun-Yan; Wei, Xian-Yong; Zhao, Yun-Peng; Cao, Jing-Pei

    2016-07-01

    Dongming lignite was sequentially extracted with petroleum ether, carbon disulfide, methanol, acetone, and isometric carbon disulfide/acetone mixed solvent at room temperature to afford extracts 1-5, respectively. High-performance liquid chromatography coupled with electrospray ionization time-of-flight mass spectrometry was used to separate and characterize heteroatomic species in the extracts at molecular level. Molecular mass of compounds in the extracts is mainly distributed from 300 to 800 u, and the relative abundance of compounds with molecular mass over 800 u in the carbon disulfide extract is 135 times of that in the petroleum ether extract. The acetone extract has the highest relative abundance for organonitrogen compounds. Double bond equivalence numbers of detected species indicate that most of the organonitrogen compounds contain N-heterocyclic aromatic rings, including pyridine, quinoline and pyrrole. Some organonitrogen isomers in Dongming lignite were separated and identified by high-performance liquid chromatography coupled with electrospray ionization time-of-flight mass spectrometry, and the corresponding structural information was proposed.

  20. 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...

  1. 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

  2. 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

  3. 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

  4. 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.

  5. Chemical characterization of aromatic compounds in extra heavy gas oil by comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry.

    Science.gov (United States)

    Avila, Bárbara M F; Pereira, Ricardo; Gomes, Alexandre O; Azevedo, Débora A

    2011-05-27

    Comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC-TOFMS) was used for the characterization of aromatic compounds present in extra heavy gas oil (EHGO) from Brazil. Individual identification of EHGO compounds was successfully achieved in addition to group-type separation on the chromatographic plane. Many aromatic hydrocarbons, especially polycyclic aromatic hydrocarbons and sulfur compounds, were detected and identified, such as chrysenes, phenanthrenes, perylenes, benzonaphthothiophenes and alkylbenzonaphthothiophenes. In addition, triaromatic steroids, methyl-triaromatic steroids, tetrahydrochrysenes and tetraromatic pentacyclic compounds were present in the EHGO aromatic fractions. Considering the roof-tile effect observed for many of these compound classes and the high number of individual compounds identified, GC×GC-TOFMS is an excellent technique to characterize the molecular composition of the aromatic fraction from EHGO samples. Moreover, data processing allowed the quantification of aromatic compounds, in class and individually, using external standards. EHGO data were obtained in μgg(-1), e.g., benzo[a]pyrene were in the range 351 to 1164μgg(-1). Thus, GC×GC-TOFMS was successfully applied in EHGO quantitative analysis.

  6. 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

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

    Science.gov (United States)

    Islam, Ananna; Kim, Donghwi; Yim, Un Hyuk; Shim, Won Joon; Kim, Sunghwan

    2015-10-15

    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.

  8. The detection and mapping of the spatial distribution of insect defense compounds by desorption atmospheric pressure photoionization Orbitrap mass spectrometry.

    Science.gov (United States)

    Rejšek, Jan; Vrkoslav, Vladimír; Hanus, Robert; Vaikkinen, Anu; Haapala, Markus; Kauppila, Tiina J; Kostiainen, Risto; Cvačka, Josef

    2015-07-30

    Many insects use chemicals synthesized in exocrine glands and stored in reservoirs to protect themselves. Two chemically defended insects were used as models for the development of a new rapid analytical method based on desorption atmospheric pressure photoionization-mass spectrometry (DAPPI-MS). The distribution of defensive chemicals on the insect body surface was studied. Since these chemicals are predominantly nonpolar, DAPPI was a suitable analytical method. Repeatability of DAPPI-MS signals and effects related to non-planarity and roughness of samples were investigated using acrylic sheets uniformly covered with an analyte. After that, analytical figures of merit of the technique were determined. The spatial distribution of (E)-1-nitropentadec-1-ene, a toxic nitro compound synthesized by soldiers of the termite Prorhinotermes simplex, was investigated. Then, the spatial distribution of the unsaturated aldehydes (E)-hex-2-enal, (E)-4-oxohex-2-enal, (E)-oct-2-enal, (E,E)-deca-2,4-dienal and (E)-dec-2-enal was monitored in the stink bug Graphosoma lineatum. Chemicals present on the body surface were scanned along the median line of the insect from the head to the abdomen and vice versa, employing either the MS or MS(2) mode. In this fast and simple way, the opening of the frontal gland on the frons of termite soldiers and the position of the frontal gland reservoir, extending deep into the abdominal cavity, were localized. In the stink bug, the opening of the metathoracic scent glands (ostiole) on the ventral side of the thorax as well as the gland reservoir in the median position under the ventral surface of the anterior abdomen were detected and localized. The developed method has future prospects in routine laboratory use in life sciences.

  9. 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.

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

    DEFF Research Database (Denmark)

    Kjeldsen, Frank; Haselmann, Kim F; Sørensen, Esben Skipper;

    2003-01-01

    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 isom......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...... such acquisitions. Unlike the case of high-energy collision-induced dissociation, no d ions were observed in the HECD of tryptic peptides....

  11. 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

  12. 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

  13. Determination of Wastewater Compounds in Whole Water by Continuous Liquid-Liquid Extraction and Capillary-Column Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Zaugg, Steven D.; Smith, Steven G.; Schroeder, Michael P.

    2006-01-01

    A method for the determination of 69 compounds typically found in domestic and industrial wastewater is described. The method was developed in response to increasing concern over the impact of endocrine-disrupting chemicals on aquatic organisms in wastewater. This method also is useful for evaluating the effects of combined sanitary and storm-sewer overflow on the water quality of urban streams. The method focuses on the determination of compounds that are indicators of wastewater or have endocrine-disrupting potential. These compounds include the alkylphenol ethoxylate nonionic surfactants, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclic aromatic hydrocarbons, and high-use domestic pesticides. Wastewater compounds in whole-water samples were extracted using continuous liquid-liquid extractors and methylene chloride solvent, and then determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-water samples fortified at 0.5 microgram per liter averaged 72 percent ? 8 percent relative standard deviation. The concentration of 21 compounds is always reported as estimated because method recovery was less than 60 percent, variability was greater than 25 percent relative standard deviation, or standard reference compounds were prepared from technical mixtures. Initial method detection limits averaged 0.18 microgram per liter. Samples were preserved by adding 60 grams of sodium chloride and stored at 4 degrees Celsius. The laboratory established a sample holding-time limit prior to sample extraction of 14 days from the date of collection.

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

    Energy Technology Data Exchange (ETDEWEB)

    Randon, J., E-mail: randon@univ-lyon1.fr [ISA Institut des Sciences Analytiques, Université Claude Bernard Lyon 1, 5 rue de la Doua, 69100 Villeurbanne (France); Maret, L. [ISA Institut des Sciences Analytiques, Université Claude Bernard Lyon 1, 5 rue de la Doua, 69100 Villeurbanne (France); Ferronato, C. [IRCELYON Institut de recherches sur la catalyse et l’environnement de Lyon, Université Claude Bernard Lyon1, 2 avenue Albert Einstein, 69626 Villeurbanne (France)

    2014-02-17

    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.

  15. 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

  16. 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

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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;

    2013-01-01

    in heteromultimeric protein complexes poses a challenge for the method due to the increased complexity of the mixture of peptides originating from all interaction partners in the complex. Previously, interference of peptides from one interaction partner has been removed by immobilizing the intact protein on beads...... 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...

  2. Soft ionization of saturated hydrocarbons, alcohols and nonpolar compounds by negative-ion direct analysis in real-time mass spectrometry.

    Science.gov (United States)

    Cody, Robert B; Dane, A John

    2013-03-01

    Large polarizable n-alkanes (approximately C18 and larger), alcohols, and other nonpolar compounds can be detected as negative ions when sample solutions are injected directly into the sampling orifice of the atmospheric pressure interface of the time-of-flight mass spectrometer with the direct analysis in real time (DART) ion source operating in negative-ion mode. The mass spectra are dominated by peaks corresponding to [M + O2]‾(•). No fragmentation is observed, making this a very soft ionization technique for samples that are otherwise difficult to analyze by DART. Detection limits for cholesterol were determined to be in the low nanogram range.

  3. Bioactive compounds of fourth generation gamma-irradiated Typhoniumflagelliforme Lodd. mutants based on gas chromatography-mass spectrometry

    Science.gov (United States)

    Sianipar, N. F.; Purnamaningsih, R.; Rosaria

    2016-08-01

    Rodent tuber (Typhonium flagelliforme Lodd.) is an Indonesian anticancer medicinal plant. The natural genetic diversity of rodent tuber is low due to vegetative propagation. Plant's genetic diversity has to be increased for obtaining clones which contain a high amount of anticancer compounds. In vitro calli were irradiated with 6 Gy of gamma ray to produce in vitro mutant plantlets. Mutant plantlets were acclimated and propagated in a greenhouse. This research was aimed to identify the chemical compounds in the leaves and tubers ofthe fourth generation of rodent tuber's vegetative mutant clones (MV4) and control plantsby using GC- MS method. Leaves and tubers of MV4 each contained 2 and 5 anticancer compounds which quantities were higher compared to control plants. MV4 leaves contained 5 new anticancer compounds while its tubers contained 3 new anticancer compounds which were not found in control. The new anticancer compounds in leaves were hexadecanoic acid, stigmast-5-en-3-ol, ergost-5-en-3-ol, farnesol isomer a, and oleic acid while the new anticancer compounds in tubers were alpha tocopherol, ergost-5-en-3-ol, and beta-elemene. Rodent tuber mutant clones are very potential to be developed into anticancer drugs.

  4. 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.

  5. 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

  6. 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

  7. 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...

  8. 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...

  9. 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.

  10. 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

  11. Characterization of volatile organic compounds (VOCs in Asian and North American pollution plumes during INTEX-B: identification of specific Chinese air mass tracers

    Directory of Open Access Journals (Sweden)

    B. Barletta

    2009-03-01

    Full Text Available 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 masses, we focused on characterizing the VOC composition of these different pollution plumes. The Chinese and other Asian air masses were significantly enhanced in carbonyl sulfide (OCS and methyl chloride (CH3Cl, while all CFC replacement compounds were elevated in US plumes, particularly HCFC-134a.

    Although elevated mixing ratios of Halon-1211 were measured in some of the Chinese plumes, several measurements at background levels were also observed. After analyzing the VOC distribution in the Chinese pollution plumes and the correlations among selected compounds, we suggest the use of a suite of species, rather than the use of a single gas, to be used as specific tracers of Chinese air masses (namely OCS, CH3Cl, 1,2-dichloroethane, and Halon-1211. In an era of constantly changing halocarbon usage patterns, this suite of gases best reflects new emission characteristics from China.

  12. 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.

  13. 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

  14. 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

  15. 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

  16. Determination of volatile aroma compounds of Ganoderma lucidum by gas chromatography mass spectrometry (HS-GC/MS).

    Science.gov (United States)

    Taşkın, Hatıra; Kafkas, Ebru; Çakıroğlu, Özgün; Büyükalaca, Saadet

    2013-01-01

    This study was conducted at Horticulture Department of Cukurova University, Adana, Turkey during 2010-2011. Fresh sample of Ganoderma lucidum collected from Mersin province of Turkey was used as material. Volatile aroma compounds were performed by Headspace Gas Chromatography (HS-GC/MS). Alcohols, aldehydes, acids, phenol, L-Alanine, d-Alanine, 3Methyl, 2-Butanamine, 2-Propanamine were determined. 1-Octen-3-ol (Alcohol) and 3-methyl butanal (Aldehyde) were identified as major aroma compounds.

  17. 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.

  18. 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.

  19. 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.

  20. An exploratory comparative study of volatile compounds in exhaled breath and emitted by skin using selected ion flow tube mass spectrometry.

    Science.gov (United States)

    Turner, Claire; Parekh, Bhavin; Walton, Christopher; Spanel, Patrik; Smith, David; Evans, Mark

    2008-01-01

    Selected ion flow tube mass spectrometry (SIFT-MS) has been used to carry out a pilot parallel study on five volunteers to determine changes occurring in several trace compounds present in exhaled breath and emitted from skin into a collection bag surrounding part of the arm, before and after ingesting 75 g of glucose in the fasting state. SIFT-MS enabled real-time quantification of ammonia, methanol, ethanol, propanol, formaldehyde, acetaldehyde, isoprene and acetone. Following glucose ingestion, blood glucose and trace compound levels were measured every 30 min for 2 h. All the above compounds, except formaldehyde, were detected at the expected levels in exhaled breath of all volunteers; all the above compounds, except isoprene, were detected in the collection bag. Ammonia, methanol and ethanol were present at lower levels in the bag than in the breath. The aldehydes were present at higher levels in the bag than in breath. The blood glucose increased to a peak about 1 h post-ingestion, but this change was not obviously correlated with temporal changes in any of the compounds in breath or emitted by skin, except for acetone. The decrease in breath acetone was closely mirrored by skin-emitted acetone in three volunteers. Breath and skin acetone also clearly change with blood glucose and further work may ultimately enable inferences to be drawn of the blood glucose concentration from skin or breath measurements in type 1 diabetes. PMID:18215004

  1. 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.

  2. 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)

  3. Environmental screening of acidic compounds based on capillary zone electrophoresis/laser-induced fluorescence detection with identification by gas chromatography/mass spectrometry and gas chromatography/high-resolution mass spectrometry.

    Science.gov (United States)

    Brumley, W C; Grange, A H; Kelliher, V; Patterson, D B; Montcalm, A; Glassman, J; Farley, J W

    2000-01-01

    This paper describes the application of capillary zone electrophoresis/laser-induced fluorescence detection (CZE/LIF) to the discovery of acidic compounds in environmental matrixes or the screening of extracts for acidic components. Published studies indicate that coal-derived materials contain a significant fraction of acidic compounds relative to materials derived from petroleum and shales. Such compounds may be useful as marker compounds for site assessment and source apportionment issues, and their identification may be important in toxicological and other health issues. We used deep-UV light from the frequency-doubled Ar ion laser at 244 and 257 nm to study extracts of samples. The CZE/LIF technique possesses good sensitivity and therefore overcomes one of the limitations of CZE with UV detection. The present work depends on high pressure/temperature solvent extraction of polynuclear aromatic hydrocarbon (PNA)-contaminated soil, followed by separation using CZE. The anionic analytes were separated by using borate or phosphate buffer (pH 9.2-12.3) after a chemical class separation. Samples were also characterized by gas chromatography/mass spectrometry (GC/MS) using full scans at low resolution, and elemental compositions were determined unequivocally by GC/high-resolution MS (GC/HRMS) using mass peak profiling (MPP). The similarity of low-resolution electron ionization mass spectra for a standard, 1-hydroxypyrene, and for a series of compounds in a contaminated-soil extract suggested that several types of phenolic and hydroxy-PNAs were present, including hydroxylated derivatives of fluorenes, fluoranthenes, and pyrenes. GC/HRMS using MPP confirmed the elemental compositions of the hydroxyfluorenes and hydroxypyrenes (and presumably hydroxyfluoranthenes) as [C13H10O] and [C16H10O], respectively. A new version of the MPP software was written for the Finnigan-MAT 900S-Trap and was similar to that developed previously for the VG 250SE. Inclusion of a calibration

  4. 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)

    Ruan, E D; Aalhus, J L; Summerfelt, S T; Davidson, J; Swift, B; Juárez, M

    2013-12-20

    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). MIB and GSM were solid phase extracted using polydimethylsiloxane (PDMS) coated stir bars, analyzed by gas chromatography, and detected in full scan mode of mass selective detector (MSD). Using this method, the calibration curves of MIB and GSM were linear in the range of 0.3-100ng/L, with a correlation coefficient above 0.999 and RSDs less than 4% (n=4). The limit of detection (LOD, S/N=3, n=6) and limit of quantification (LOQ, S/N=10, n=6) of MIB and GSM were both ∼0.3 and 1ng/L, respectively. The recoveries of MIB and GSM were 22% and 29% by spike in 30ng/L standard compounds, 23% and 30% by spike-in 100ng/L standard compounds in salmon tissue samples with good precision (<8% of RSDs, n=6), respectively. The recoveries of MIB and GSM were better than reported methodologies using SPME fibres (<10%) in fish tissue samples. This method was successfully applied to monitor and characterize depurated salmon fillet samples (0, 3, 6 and 10 days).

  5. 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

  6. 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

  7. 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

  8. A validated ultra-high performance liquid chromatography coupled to high resolution mass spectrometry analysis for the simultaneous quantification of the three known boar taint compounds.

    Science.gov (United States)

    Bekaert, K M; Vanden Bussche, J; François, S; Tuyttens, F A M; De Brabander, H F; Vandendriessche, F; Vanhaecke, L

    2012-05-25

    Boar taint is an off-odour that can occur when meat or fat from entire male pigs is heated. Most of the currently available analytical methods are not capable of detecting the three known boar taint compounds (indole, skatole and androstenone) simultaneously, which renders their analysis often labour-intensive and time-consuming as separate analyses are required. In this study a validated U-HPLC-HR-Orbitrap-MS analysis method is described for the quantitative determination of the three boar taint compounds in fat. The sample pre-treatment involves a melting step followed by extraction with methanol and clean-up consisting of a freezing step and solid phase extraction (HLB cartridges). The analytes are then chromatographically separated and detected with an Exactive high-resolution mass spectrometer. Due to the absence of guidelines for the analysis of boar taint in fat, the Commission Decision 2002/657/EC [18] and ISO 17025 [19] guidelines were used as guideline for validation of the developed detection method. This resulted in limits of detection and limits of quantification between 2.5 and 7 μg kg(-1) and between 5 and 10 μg kg(-1) for the three compounds, respectively, which is far below the threshold values set at 100 μg L(-1) for indole, 200 μg L(-1) for skatole and 1000 μg L(-1) for androstenone in pig fat samples. The method obtained for the three compounds a repeatability (RSD) lower then 12.7% and a within-laboratory reproducibility (RSD) lower than 16.9%. The recovery of the three compounds ranged between 99 and 112 and an excellent linearity (R(2) ≥ 0.99) was found. In the future, this method may be extended with other compounds that turn out to be correlated with boar taint. PMID:22498353

  9. 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

  10. 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.

  11. Characterization of volatile organic compounds (VOCs in Asian and north American pollution plumes during INTEX-B: identification of specific Chinese air mass tracers

    Directory of Open Access Journals (Sweden)

    A. J. Weinheimer

    2009-07-01

    Full Text Available 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 masses we characterized their VOC composition and we compared their background levels with those obtained during the 2004 INTEX-A mission. The Chinese and other Asian air masses were significantly enhanced in carbonyl sulfide (OCS and methyl chloride (CH3Cl, while all CFC replacement compounds were elevated in US plumes, particularly HFC-134a.

    Although elevated mixing ratios of Halon-1211 were measured in some Chinese plume samples, several measurements at background levels were also observed. After analyzing the VOC distribution and correlations within the Chinese pollution plumes and applying principal component analysis (PCA, we suggest the use of a suite of species, rather than a single gas, as specific tracers of Chinese air masses (namely OCS, CH3Cl, 1,2-dichloroethane, ethyl chloride, and Halon-1211. In an era of constantly changing halocarbon usage patterns, this suite of gases best reflects new emission characteristics from China.

  12. 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

  13. 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

  14. Identification of potentially toxic compounds in complex extracts of environmental samples using gas chromatography-mass spectrometry and multivariate data analysis.

    Science.gov (United States)

    Bergknut, Magnus; Kucera, Adam; Frech, Kristina; Andersson, Erika; Engwall, Magnus; Rannug, Ulf; Koci, Vladimir; Andersson, Patrik L; Haglund, Peter; Tysklind, Mats

    2007-02-01

    In this study, we examined 31 samples of varying chemical composition, including samples of soils from gasworks, coke production sites, and sites where wood preservatives were heavily used; ash and soot from municipal solid waste incinerators; antiskid sand; and dust from areas with heavy road traffic. The samples were comprehensively chemically characterized, especially their polycyclic aromatic compound contents, using gas chromatography-time-of-flight mass spectrometry, whereas their biological effects were assessed using dehydrogenase activity, root growth (Hordeum vulgare), reproduction of springtails (Folsomia candida), algal growth (Desmodesmus subspicatus), germinability (Sinapis alba), Vibrio fischeri, DR-CALUX, and Ames Salmonella assays. The number of compounds detected in the samples ranged from 123 to 527. Using the multivariate regression technique of partial-least-squares projections to latent structures, it was possible to find individual compounds that exhibited strong correlations with the different biological responses. Some of the results, however, indicate that a broader chemical characterization may be needed to identify all the compounds that may cause the measured biological responses.

  15. 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

  16. Development of a fast extraction method and optimization of liquid chromatography-mass spectrometry for the analysis of phenolic compounds in lentil seed coats.

    Science.gov (United States)

    Mirali, Mahla; Ambrose, Stephen J; Wood, Stephen A; Vandenberg, Albert; Purves, Randy W

    2014-10-15

    A systematic set of optimization experiments was conducted to design an efficient extraction and analysis protocol for screening six different sub-classes of phenolic compounds in the seed coat of various lentil (Lens culinaris Medik.) genotypes. Different compounds from anthocyanidins, flavan-3-ols, proanthocyanidins, flavanones, flavones, and flavonols sub-classes were first optimized for use as standards for liquid chromatography mass spectrometry (LC-MS) with UV detection. The effect of maceration duration, reconstitution solvent, and extraction solvent were investigated using lentil genotype CDC Maxim. Chromatographic conditions were optimized by examining column separation efficiencies, organic composition, and solvent gradient. The results showed that a 1h maceration step was sufficient and that non-acidified solvents were more appropriate; a 70:30 acetone: water (v/v) solvent was ultimately selected. Using a Kinetex PFP column, the organic concentration, gradient, and flow rate were optimized to maximize the resolution of phenolic compounds in a short 30-min analysis time. The optimized method was applied to three lentil genotypes with different phenolic compound profiles to provide information of value to breeding programs.

  17. 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.

  18. 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

  19. Speciation of nitrogen-containing compounds in an unfractionated coal tar sample by comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry.

    Science.gov (United States)

    da Silva, Juliana M; Machado, Maria Elisabete; Maciel, Gabriela P S; Dal Molin, Daniela; Caramão, Elina B

    2014-12-19

    Comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC/TOFMS) has shown great skill in analyzing complex mixtures such as fossil fuels, especially for compounds at low concentrations. The analysis of N-polyaromatic compounds (NPAC) in coal and crude oil is a great challenge for analytical chemistry due to its environmental and technological importance, and also its diversity of concentration in the matrix. This study is the first report in the applicability of GC×GC/TOFMS for detection of NPAC in a coal tar sample with no fractionation. Normally these compounds are analyzed after sample treatment, making the process expensive and time consuming. However, the higher separation power of GC×GC/TOFMS, compared to 1D-GC, produces cleaner mass spectra in complex samples, which helps in identification of analytes with no pre-fractionation. In this paper, the main objectives were to demonstrate the applicability of GC×GC/TOFMS in the speciation and separation between basic and neutral NPAC from coal tar sample derived from fast pyrolysis, without prior sample fractionation. The methodology used here consisted of chromatographic injection of the diluted sample using a conventional columns set and data analysis by ChromaTOF/Excel™ software. Some basic compounds (pyridines and quinolines) and neutral ones (carbazoles and indoles) were detected with good chromatographic separation and spectral similarity. Tools like spectral deconvolution, extracted ion chromatogram (EIC) and dispersion graphics allowed greater security on the identification and separation of NPAC in this complex sample of coal tar, with no pre-treatment.

  20. 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

  1. 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

  2. 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

  3. 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

  4. 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...... to 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...

  5. 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)

  6. 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

  7. 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.

  8. 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 ch...

  9. 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.

  10. The EPA iCSS Chemistry Dashboard to Support Compound Identification Using High Resolution Mass Spectrometry Data (ACS Fall meeting)

    Science.gov (United States)

    Abstract: There is a growing need for rapid chemical screening and prioritization to inform regulatory decision-making on thousands of chemicals in the environment. We have previously used high-resolution mass spectrometry to examine household vacuum dust samples using liquid chr...

  11. 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

  12. [Simultaneous determination of multi-organotin compounds in seawater by liquid-liquid extraction-high performance liquid chromatography-inductively coupled plasma mass spectrometry].

    Science.gov (United States)

    Yu, Zhen-Hua; Jing, Miao; Wang, Xiao-Ru; Chen, Deng-Yun; Huang, Yan-Liang

    2009-10-01

    The hyphenated technique of high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry (HPLC-ICP-MS) was applied to the simultaneous determination of five organotin compounds (trimethyltin, dibutyltin, tributyltin, diphenyltin and triphenyltin) in seawater samples. Agilent TC-C18 column was used for the separation, the mobile phase of HPLC was CH3CN : H2O : CH3COOH = 65 : 23 : 12 (phi3), 0.05% TEA, and pH value was adjusted to 3.0 by diluent ammonia. The flow rate was 0.6 mL x min(-1). Five mixed organotin compounds in a mix standard solution from 100 to 0.5 microg x L(-1) were applied for the method assessment. The experimental results indicate that the correlation coefficient of calibration curves (R2) for each organotin compound was over 0.998 and the detection limits of the five organotin compounds were lower than 3 ng x L(-1). Different mixed organic solvents including dichloromethane or toluene were used for extraction of organotin and the extraction condition of organotin from seawater was optimized. The 100 mL seawater acidized by hydrochloric acid was extracted by 10 mL carbon dichloride (CH2 Cl2) with 2% tropolone for 10 min twice. Extracted organic solvents were mixed and blown to one drop by nitrogen with the rate of 1.7 mL x min(-1), then 1 mL acetonitrile was added to the drop for redissolving the organotin compounds. Finally, the mixed redissolution was filtered by 0.22 microm organic filter membrane before analysis. It was found that the only organotin compound in seawater was triphenyltin (TPHT) and the content was 53.2 ng x L(-1). The recoveries test from the standard addition for diphenyltin (DPHT), dibutyltin (DBT), tributyltin (TBT) and triphenyltin (TPHT) were over 80%. However, the recovery for trimethyltin (TMT) was relatively low and the value was 50%. The reason might be attributed to the decomposition or adsorption of those compounds during the extraction procedure. Further study on this subject is in

  13. 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

  14. 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.

  15. 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)

  16. 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...

  17. Compound-specific carbon isotopes from Earth's largest flood basalt eruptions directly linked to the end-Triassic mass extinction.

    Science.gov (United States)

    Whiteside, Jessica H; Olsen, Paul E; Eglinton, Timothy; Brookfield, Michael E; Sambrotto, Raymond N

    2010-04-13

    A leading hypothesis explaining Phanerozoic mass extinctions and associated carbon isotopic anomalies is the emission of greenhouse, other gases, and aerosols caused by eruptions of continental flood basalt provinces. However, the necessary serial relationship between these eruptions, isotopic excursions, and extinctions has never been tested in geological sections preserving all three records. The end-Triassic extinction (ETE) at 201.4 Ma is among the largest of these extinctions and is tied to a large negative carbon isotope excursion, reflecting perturbations of the carbon cycle including a transient increase in CO(2). The cause of the ETE has been inferred to be the eruption of the giant Central Atlantic magmatic province (CAMP). Here, we show that carbon isotopes of leaf wax derived lipids (n-alkanes), wood, and total organic carbon from two orbitally paced lacustrine sections interbedded with the CAMP in eastern North America show similar excursions to those seen in the mostly marine St. Audrie's Bay section in England. Based on these results, the ETE began synchronously in marine and terrestrial environments slightly before the oldest basalts in eastern North America but simultaneous with the eruption of the oldest flows in Morocco, a CO(2) super greenhouse, and marine biocalcification crisis. Because the temporal relationship between CAMP eruptions, mass extinction, and the carbon isotopic excursions are shown in the same place, this is the strongest case for a volcanic cause of a mass extinction to date.

  18. 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

  19. 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.

  20. Effects of conventional heating on the stability of major olive oil phenolic compounds by tandem mass spectrometry and isotope dilution assay.

    Science.gov (United States)

    Attya, Mohamed; Benabdelkamel, Hicham; Perri, Enzo; Russo, Anna; Sindona, Giovanni

    2010-01-01

    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. PMID:21124271

  1. 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.

  2. 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

  3. 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.

  4. 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 ...

  5. 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.

  6. Development of a fast liquid chromatography-tandem mass spectrometry method for the determination of endocrine-disrupting compounds in waters.

    Science.gov (United States)

    Di Carro, Marina; Scapolla, Carlo; Liscio, Camilla; Magi, Emanuele

    2010-09-01

    A fast liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS-MS) method was developed to study five endocrine-disrupting compounds (4-n-nonylphenol, bisphenol A, estrone, 17β-estradiol and 17α-ethinylestradiol) in water. Different columns were tested; the chromatographic separation of the analytes was optimized on a Pinnacle DB biphenylic column with a water-acetonitrile gradient elution, which allowed the separation of the selected endocrine-disrupting compounds (EDCs) in less than 6 min. Quantitative analysis was performed in selected reaction monitoring (SRM) mode; two transitions were chosen for each compound, using the most abundant for quantitation. Calibration curves using bisphenol A-d (16) as internal standard were drawn, showing good correlation coefficients (0.9993-0.9998). All figures of merit of the method were satisfactory; limits of detection were in the low pg range for all analytes. The method was then applied to the determination of the analytes in real water samples: to this aim, polar organic chemical integrative samplers (POCIS) were deployed in the influent and in the effluent of a drinking water treatment plant in Liguria (Italy). The EDC level was rather low in the influent and negligible in the outlet, reflecting the expected function of the treatment plant.

  7. 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 (gas-to-liquid technologies from natural gas and guide the choice of an FT conversion process that generates clean products with higher added value.

  8. 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

  9. [Simultaneous determination of 23 ester compounds in cigarette water-borne adhesives by liquid-liquid extraction and gas chromatography-mass spectrometry].

    Science.gov (United States)

    Gong, Shuguo; Kong, Bo; Tuo, Suxing; Dai, Yunhui; Wu, Mingjian; Tan, Liquan; Liu, Wei

    2013-10-01

    A method of gas chromatography-mass spectrometry (GC-MS) with liquid-liquid extraction has been developed for the simultaneous determination of 23 ester compounds including acetate esters, acrylic esters, metacrylic acid esters and phthalate acid esters in cigarette water-borne adhesives. After dispersed in water, the sample was extracted by n-hexane solution containing phenyl ethyl propionate as internal standard substance. Then, the solution was centrifuged and filtrated through a 0.45 microm organic membrane filter. Finally, the solution was separated on a DB-WAXETR column (60 m x 0.25 mm x 0.25 microm), and detected with MS in selected ion monitoring mode, and quantified by internal standard method. The results showed a good linear correlation in the range of 0.4-50.0 mg/L. The recoveries of the ester compounds spiked in the sample were 81.8%-109.1%, and the relative standard deviations (RSDs, n = 5) were less than 4%. The limits of detection (LODs) and limits of quantification (LOQs were in the ranges of 0.02-0.76 mg/kg and 0.04-2.52 mg/kg, respectively. The method is simple, time-saving, and has high sensitivity and good reproducibility. It can be applied to the determination of the 23 ester compounds in cigarette water-borne adhesives.

  10. 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.

  11. 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.

  12. 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

  13. Multivariate optimization approach for the analysis of butyltin compounds in mussel tissues by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Magi, Emanuele; Liscio, Camilla; Di Carro, Marina

    2008-11-01

    The derivatization with NaBEt(4) for the determination of butyltin compounds in mussel tissues (Mytilus galloprovincialis) by GC-MS was optimized using a central composite design. The effects of NaBEt(4) concentration, pH and acetate buffer concentration on the derivatization efficiency were considered. Solid-phase extraction with Florisil cartridges was performed, demonstrating that the clean-up drastically reduces the background and improves the sensitivity. The good accuracy of the method was verified on a certified reference material (ERM 477); the figures of merit for all the three analytes, evaluated under optimum conditions, were satisfactory. The optimized derivatization procedure was applied to the determination of the analytes in mussels exposed to tributyltin (TBT). All considered tissues showed considerable accumulation of TBT, especially gills.

  14. 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.

  15. 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

  16. Emissions and ambient distributions of Biogenic Volatile Organic Compounds (BVOC in a ponderosa pine ecosystem: interpretation of PTR-MS mass spectra

    Directory of Open Access Journals (Sweden)

    S. Kim

    2010-02-01

    Full Text Available Two proton-transfer-reaction mass spectrometry systems were deployed at the Bio-hydro-atmosphere interactions of Energy, Aerosols, Carbon, H2O, Organics and Nitrogen-Southern Rocky Mountain 2008 field campaign (BEACHON-SRM08; July to September, 2008 at the Manitou Forest Observatory in a ponderosa pine woodland near Woodland Park, Colorado USA. The two PTR-MS systems simultaneously measured BVOC emissions and ambient distributions of their oxidation products. Here, we present mass spectral analysis in a wide range of masses (m/z 40+ to 210+ to assess our understanding of BVOC emissions and their photochemical processing inside of the forest canopy. The biogenic terpenoids, 2-methyl-3-butene-2-ol (MBO, 50.2% and several monoterpenes (MT, 33.5% were identified as the dominant BVOC emissions from a transmission corrected mass spectrum (PTR-MS, averaged over the daytime (11 a.m. to 3 p.m., local time of three days. To assess contributions of oxidation products of local BVOC, we calculate an oxidation product spectrum with the OH- and ozone-initiated oxidation product distribution mass spectra of two major BVOC emissions at the ecosystem (MBO and β-pinene that were observed from laboratory oxidation experiments. The majority (~76% of the total signal in the transmission corrected PTR-MS spectra could be explained by identified compounds. The remainder are attributed to oxidation products of BVOC emitted from nearby ecosystems and transported to the site, and oxidation products of unidentified BVOC emitted from the ponderosa pine ecosystem.

  17. 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

  18. Gas phase ion-molecule reactions of buckminsterfullerene C60 with some small organic compounds in mass spectrometer

    Institute of Scientific and Technical Information of China (English)

    刘淑莹; 郭兴华; 刘子阳; 倪嘉缵

    1995-01-01

    In chemical ionization mass spectrometry (CIMS) gas phase C60+ or C60can react with fragment ions from three chloromethane and four multichloroethane molecular ions via ion-molecule reactions A dozen of gas-phase adduct ions of C60 are observed, and most of them contain chlorine atoms The results of the comparison and analysis show that the relative intensities of adduct ions are not directly proportional to the corresponding fragment ions in the MS of reagents,which implies that some fragment ions containing radicals are more reactive with C60+ or C60. This indicates that the alkene-like C60+ or C60 can act as a radical sponge in addition reactions.

  19. 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

  20. 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

  1. 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.

  2. Carbon dioxide capture using polyethylenimine-loaded mesoporous carbons.

    Science.gov (United States)

    Wang, Jitong; Chen, Huichao; Zhou, Huanhuan; Liu, Xiaojun; Qiao, Wenming; Long, Donghui; Ling, Licheng

    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 degrees C, 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 degrees C, 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.

  3. 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

  4. 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

  5. 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.

  6. Determination of organotin compounds in-water by headspace solid phase microextraction with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Chou, Chi-Chi; Lee, Maw-Rong

    2005-01-28

    This investigation evaluates headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) to determine trace levels of organotins in water. The organotins were derivatized in situ with sodium tetraethylborate and adsorbed on a poly(dimethysiloxane) (PDMS)-coated fused silica fiber. The SPME experimental procedures to extract organotins in water were at pH 5, with extraction and derivatization simultaneously at 45 degrees C for 30 min in a 2% sodium tetraethylborate solution and a sample solution volume in the ratio of 1:1, and desorption in the splitless injection port of the GC at 260 degrees C for 2 min. Detection limits are determined to be in the low ng/L range. According to the analysis, the linearity range is from 10 to 10,000 ng/L with R.S.D. values below 12% except triphenyltin (24%). The proposed method was tested by analyzing surface seawater from the harbors on the Taiwanese coast for organotins residues. Some organotins studied were detected in the analyzed samples. Results of this study demonstrate the adequacy of the headspace SPME-GC-MS method for analyzing organotins in sea water samples. PMID:15729814

  7. 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.

  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. 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...

  10. 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}.

  11. 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

  12. 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.

  13. 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

  14. 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.

  15. 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

  16. Profiling of compounds and degradation products from the postharvest treatment of pears and apples by ultra-high pressure liquid chromatography quadrupole-time-of-flight mass spectrometry.

    Science.gov (United States)

    Picó, Yolanda; la Farré, Marinel; Segarra, Ramon; Barceló, Damià

    2010-04-15

    This study deals with a simple strategy to pinpoint potential unknown compounds in full scan mass spectrometry (MS) experiments. Forty samples of apples and pears intended for human consumption were analyzed by ultra-high performance liquid chromatography quadrupole-time-of-flight (UPLC-QqTOF-MS), after extraction of the possible contaminants by rinsing the peel of the fruit with ethyl acetate. The peaks were visually recognized in the total ion chromatogram (TIC). Two major types of postharvest treatments were detected in this set of samples: imazalil (IMZ)/ethoxyquin (EQ) and thiabendazole (TBZ)/diphenylamine (DPA). The present work also describes the metabolites formed by degradation of EQ (to our knowledge not previously reported) and DPA (there was mass spectral evidence of some of them but full identification was not pursued). Hydroxy-DPA, n-phenyl-4-quinoneimine, methoxy-DPA, demethyl-EQ, demethyldehydro-EQ, EQ-dimer, methyl-EQ, EQ-N-oxyl and 2',2,4,-trimethyl-6-quinolone were unequivocally identified and confirmed. Some relationships between the applied postharvest treatment and the metabolites formed were established. Remarkably, they may constitute a useful fingerprint in further investigations of postharvest treatments. Among other significant results, the study also reveals for the first time the presence of some EQ metabolites in fruits, which are different from those previously reported in animal tissues. There is not information on the occurrence of EQ metabolites in fruits and the DPA ones have not been studied extensively in pears and apples. The levels of the metabolites found exceeded several times those of the parent compounds.

  17. 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

  18. 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.

  19. 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

  20. Microwave-assisted on-spot derivatization for gas chromatography-mass spectrometry based determination of polar low molecular weight compounds in dried blood spots.

    Science.gov (United States)

    Sadones, Nele; Van Bever, Elien; Archer, John R H; Wood, David M; Dargan, Paul I; Van Bortel, Luc; Lambert, Willy E; Stove, Christophe P

    2016-09-23

    Dried blood spot (DBS) sampling and analysis is increasingly being applied in bioanalysis. Although the use of DBS has many advantages, it is also associated with some challenges. E.g. given the limited amount of available material, highly sensitive detection techniques are often required to attain sufficient sensitivity. In gas chromatography coupled to mass spectrometry (GC-MS), derivatization can be helpful to achieve adequate sensitivity. Because this additional sample preparation step is considered as time-consuming, we introduce a new derivatization procedure, i.e. "microwave-assisted on-spot derivatization", to minimize sample preparation of DBS. In this approach the derivatization reagents are directly applied onto the DBS and derivatization takes place in a microwave instead of via conventional heating. In this manuscript we evaluated the applicability of this new concept of derivatization for the determination of two polar low molecular weight molecules, gamma-hydroxybutyric acid (GHB) and gabapentin, in DBS using a standard GC-MS configuration. The method was successfully validated for both compounds, with imprecision and bias values within acceptance criteria (weight compounds of interest in clinical and/or forensic toxicology, including vigabatrin, beta-hydroxybutyric acid, propylene glycol, diethylene glycol, 1,4-butanediol and 1,2-butanediol, can also be detected using this method. PMID:27578413

  1. 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.

  2. Determination of aromatic sulphur compounds in heavy gas oil by using (low-)flow modulated comprehensive two-dimensional gas chromatography-triple quadrupole mass spectrometry.

    Science.gov (United States)

    Franchina, Flavio Antonio; Machado, Maria Elisabete; Tranchida, Peter Quinto; Zini, Cláudia Alcaraz; Caramão, Elina Bastos; Mondello, Luigi

    2015-03-27

    The present research is focused on the development of a flow-modulated comprehensive two-dimensional gas chromatography-triple quadrupole mass spectrometry (FM GC × GC-MS/MS) method for the determination of classes of aromatic organic sulphur compounds (benzothiophenes, dibenzothiophenes, and benzonaphthothiophene) in heavy gas oil (HGO). The MS/MS instrument was used to provide both full-scan and multiple-reaction-monitoring (MRM) data. Linear retention index (LRI) ranges were used to define the MRM windows for each chemical class. Calibration solutions (internal standard: 1-fluoronaphthalene) were prepared by using an HGO sample, depleted of S compounds. Calibration information was also derived for the thiophene class (along with MRM and LRI data), even though such constituents were not present in the HGO. Linearity was satisfactory over the analyzed concentration range (1-100 mg/L); intra-day precision for the lowest calibration point was always below 17%. Accuracy was also satisfactory, with a maximum percentage error of 3.5% (absolute value) found among the S classes subjected to (semi-)quantification. The highest limit of quantification was calculated to be 299 μg/L (for the C1-benzothiophene class), while the lowest was 21 μg/L (for the C4-benzothiophene class).

  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. Real-time quantification of traces of biogenic volatile selenium compounds in humid air by selected ion flow tube mass spectrometry.

    Science.gov (United States)

    Sovová, Kristýna; Shestivska, Violetta; Španěl, Patrik

    2012-06-01

    Biological volatilization of selenium, Se, in a contaminated area is an economical and environmentally friendly approach to phytoremediation techniques, but analytical methods for monitoring and studying volatile compounds released in the process of phytovolatilization are currently limited in their performance. Thus, a new method for real time quantification of trace amounts of the vapors of hydrogen selenide (H(2)Se), methylselenol (CH(3)SeH), dimethylselenide ((CH(3))(2)Se), and dimethyldiselenide ((CH(3))(2)Se(2)) present in ambient air adjacent to living plants has been developed. This involves the characterization of the mechanism and kinetics of the reaction of H(3)O(+), NO(+), and O(2)(+•) reagent ions with molecules of these compounds and then use of the rate constants so obtained to determine their absolute concentrations in air by selected ion flow tube mass spectrometry, SIFT-MS. The results of experiments demonstrating this method on emissions from maize (Zea mays) seedlings cultivated in Se rich medium are also presented.

  6. Determination of mercury compounds in fish by microwave-assisted extraction and liquid chromatography-vapor generation-inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Chiou, Chwei-Sheng; Jiang, Shiuh-Jen; Kumar Danadurai, K. Suresh

    2001-07-01

    A method employing a vapor generation system and LC combined with inductively coupled plasma mass spectrometry (LC-ICP-MS) is presented for the determination of mercury in biological tissues. An open vessel microwave digestion system was used to extract the mercury compounds from the sample matrix. The efficiency of the mobile phase, a mixture of L-cysteine and 2-mercaptoethanol, was evaluated for LC separation of inorganic mercury [Hg(II)], methylmercury (methyl-Hg) and ethylmercury (ethyl-Hg). The sensitivity, detection limits and repeatability of the liquid chromatography (LC) ICP-MS system with a vapor generator were comparable to, or better than, that of an LC-ICP-MS system with conventional pneumatic nebulization, or other sample introduction techniques. The experimental detection limits for various mercury species were in the range of 0.05-0.09 ng ml -1 Hg, based on peak height. The proposed method was successfully applied to the determination of mercury compounds in a swordfish sample purchased from the local market. The accuracy of the method was evaluated by analyzing a marine biological certified reference material (DORM-2, NRCC).

  7. Identification of compounds from high-fat and extra virgin olive oil-supplemented diets in whole mouse liver extracts and isolated mitochondria using mass spectrometry.

    Science.gov (United States)

    dos Santos, Gustavo Aparecido; Ferreira, Mônica Siqueira; de Oliveira, Diogo Noin; de Oliveira, Vanessa; Siqueira-Santos, Edilene S; Cintra, Dennys Esper Corrêa; Castilho, Roger Frigério; Velloso, Lício Augusto; Catharino, Rodrigo Ramos

    2015-07-01

    Nonalcoholic steatohepatitis (NASH) is a fatty liver disorder that could be improved with extra virgin olive oil (EVOO) supplementation in diet. We propose the monitoring, in whole mouse liver extracts and in isolated mitochondria, of the absorption of compounds from three different diets: standard (CT), high-fat (HFD) and high-fat supplemented with EVOO (HFSO). Male mice were submitted to one of the following three diets: CT or HFD for 16 weeks or HFD for 8 weeks followed by additional 8 weeks with HFSO. Following this period, liver was extracted for histological evaluation, mitochondria isolation and mass spectrometry analyses. Diets, liver extracts and Percoll-purified mitochondria were analyzed using ESI-MS and the lipidomics approach. Morphological, histological and spectrometric results indicated a decrease in NASH severity with EVOO supplementation in comparison with animals maintained with HFD. Spectrometric data also demonstrated that some compounds presented on the diets are absorbed by the mitochondria. EVOO was shown to be a potential therapeutic alternative in food for NASH. Our results are in accordance with the proposition that the major factor that influences different responses to diets is their composition - and not only calories - especially when it comes to studies on obesity.

  8. First results on headspace-solid phase microextraction-gas chromatography/mass spectrometry of volatile organic compounds emitted by wax objects in museums.

    Science.gov (United States)

    Lattuati-Derieux, A; Thao, S; Langlois, J; Regert, M

    2008-04-11

    Sampling volatile organic compounds (VOCs) emitted by a large variety of materials is nowadays a very useful technique for analytical purpose. In the field of cultural heritage, it can be applied to identify some constituents of museum artefacts off-gassing VOCs without sampling on the object itself. In this study, we focused on objects made of wax. First volatiles emitted by a reference beeswax were trapped and identified by headspace-solid phase microextraction (HS-SPME)-gas chromatography and mass spectrometry (GC/MS). This allowed to identify numerous volatile biomarkers, namely saturated n-alkanes from C(10) to C(21), saturated n-carboxylic acids containing 6-12 carbon atoms, benzene and cinnamic derivatives that may be considered as volatile biomarkers of beeswax. The SPME strategy was then performed at the Orsay museum (Paris) in a showcase containing a wax sculpture "Le Mineur de la Loire" by J.-J. Carriès. The use of beeswax in this sculpture was unequivocally confirmed by the VOCs concentrated in the showcase, together with a set of characteristic molecular compounds identified by HT-GC/MS. HS-SPME-GC/MS thus appears to be a powerful in situ and non-invasive analytical technique that allows to identify natural substances in the field of cultural heritage without any sampling of solid matter from the object. The results obtained are promising for orientating the strategy of preventive conservation related to works of art characterised by important emission of VOCs.

  9. Simultaneous Determination of Perfluorinated Compounds in Edible Oil by Gel-Permeation Chromatography Combined with Dispersive Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry.

    Science.gov (United States)

    Yang, Lili; Jin, Fen; Zhang, Peng; Zhang, Yanxin; Wang, Jian; Shao, Hua; Jin, Maojun; Wang, Shanshan; Zheng, Lufei; Wang, Jing

    2015-09-30

    A simple analytical method was developed for the simultaneous analysis of 18 perfluorinated compounds (PFCs) in edible oil. The target compounds were extracted by acetonitrile, purified by gel permeation chromatography (GPC) and dispersive solid-phase extraction (DSPE) using graphitized carbon black (GCB) and octadecyl (C18), and analyzed by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ES-MS/MS) in negative ion mode. Recovery studies were performed at three fortification levels. The average recoveries of all target PFCs ranged from 60 to 129%, with an acceptable relative standard deviation (RSD) (1-20%, n = 3). The method detection limits (MDLs) ranged from 0.004 to 0.4 μg/kg, which was significantly improved compared with the existing liquid-liquid extraction and cleanup method. The method was successfully applied for the analysis of all target PFCs in edible oil samples collected from markets in Beijing, China, and the results revealed that C6-C10 perfluorocarboxylic acid (PFCAs) and C7 perfluorosulfonic acid PFSAs were the major PFCs detected in oil samples.

  10. 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

  11. 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

    2015-02-05

    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.

  12. 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

  13. 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

  14. 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.

  15. 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

  16. 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.

  17. Atmospheric mass deposition by captured planetesimals

    Science.gov (United States)

    Iaroslavitz, Eyal; Podolak, Morris

    2007-04-01

    We examine the deposition of heavy elements in the envelope of a protoplanet growing according to the core accretion scenario of Pollack et al. [Pollack, J.B., Hubickyj, O., Bodenheimer, P., Lissauer, J.J., Podolak, M., Greenzweig, Y., 1996. Icarus 124, 62-85]. We use their atmospheric models and the deposition rates that they computed, and we calculate the amount of heavy elements that can be dissolved in the envelope. For planetesimals composed of a mixture of water, CHON, and rock, we find that almost all of the water is dissolved in the atmosphere. A substantial amount of CHON is also dissolved but it remains sequestered at high temperatures near the core. Some fraction of the rock is also dissolved in the very high temperature region near the core envelope boundary. If this dissolved material can be mixed upward later in the planet's evolution, the resulting structure would be much closer to that determined by matching the moments of Jupiter's gravitational field.

  18. 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...

  19. Experimental Evaluation of the Effect of Angle-of-attack on the External Aerodynamics and Mass Capture of a Symmetric Three-engine Air-breathing Launch Vehicle Configuration at Supersonic Speeds

    Science.gov (United States)

    Kim, Hyun D.; Frate, Franco C.

    2001-01-01

    A subscale aerodynamic model of the GTX air-breathing launch vehicle was tested at NASA Glenn Research Center's 10- by 10-Foot Supersonic Wind Tunnel from Mach 2.0 to 3.5 at various angles-of-attack. The objective of the test was to investigate the effect of angle-of-attack on inlet mass capture, inlet diverter effectiveness, and the flowfield at the cowl lip plane. The flow-through inlets were tested with and without boundary-layer diverters. Quantitative measurements such as inlet mass flow rates and pitot-pressure distributions in the cowl lip plane are presented. At a 3deg angle-of-attack, the flow rates for the top and side inlets were within 8 percent of the zero angle-of-attack value, and little distortion was evident at the cowl lip plane. Surface oil flow patterns showing the shock/boundary-layer interaction caused by the inlet spikes are shown. In addition to inlet data, vehicle forebody static pressure distributions, boundary-layer profiles, and temperature-sensitive paint images to evaluate the boundary-layer transition are presented. Three-dimensional parabolized Navier-Stokes computational fluid dynamics calculations of the forebody flowfield are presented and show good agreement with the experimental static pressure distributions and boundary-layer profiles. With the boundary-layer diverters installed, no adverse aerodynamic phenomena were found that would prevent the inlets from operating at the required angles-of-attack. We recommend that phase 2 of the test program be initiated, where inlet contraction ratio and diverter geometry variations will be tested.

  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. 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.)

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

    Energy Technology Data Exchange (ETDEWEB)

    Xu Ting [College of Resources and Environmental Sciences, China Agricultural University, Beijing 100193 (China); Department of Molecular Biosciences and Bioengineering, University of Hawaii at Manoa, 1955 East-West Road, Honolulu, HI 96822 (United States); Cho, Il Kyu; Wang Dongli [Department of Molecular Biosciences and Bioengineering, University of Hawaii at Manoa, 1955 East-West Road, Honolulu, HI 96822 (United States); Rubio, Fernando M. [Abraxis LLC, 54 Steamwhistle Drive, Warminster, PA 18974 (United States); Shelver, Weilin L. [USDA-ARS Biosciences Research Laboratory, 1605 Albrecht Boulevard, Fargo, ND 58105 (United States); Gasc, Anne M.E. [Encore, Inc., P.O. Box 47, Waimanalo, HI 96795-0047 (United States); Li, Ji [College of Resources and Environmental Sciences, China Agricultural University, Beijing 100193 (China); Li, Qing X. [Department of Molecular Biosciences and Bioengineering, University of Hawaii at Manoa, 1955 East-West Road, Honolulu, HI 96822 (United States)], E-mail: qingl@hawaii.edu

    2009-02-15

    A gas chromatograph/electron capture detector-ion trap mass spectrometer (GC/ECD-ITMS) was used for the determination of polybrominated diphenyl ethers (PBDEs) in euryhaline fish and crabs. GC/ECD-ITMS results showed that average recoveries from the spiked fish samples are in a range of 58-123% with relative standard deviations (RSDs) of 5-19%. PBDE concentrations obtained from GC/ECD-ITMS ranged from 28 ng/g to 1845 ng/g lipid weight (lw) in all aquatic species collected from Hawaiian brackish waters. The general BDE congener concentration profile observed in this study is BDE-47 > BDE-100 > BDE-154 > BDE-99 > BDE-153 > BDE-28 > BDE-183. The ELISA results expressed as BDE-47 equivalents correlated well with those of GC/ECD-ITMS, with a correlation coefficient (R{sup 2} = 0.68) and regression coefficient (slope = 0.82). Comparison of ELISA with GC/ECD-ITMS results demonstrated that ELISA provides a timely and cost-effective method to screen PBDEs in fish and crab samples. - PBDEs (with the most abundant being BDE-47) at concentrations of 28-1845 ng/g lipid weight in fish and crabs from Hawaiian freshwater were detected with both ELISA and GC/MS.

  3. 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.).

  4. Microwave-assisted on-spot derivatization for gas chromatography-mass spectrometry based determination of polar low molecular weight compounds in dried blood spots.

    Science.gov (United States)

    Sadones, Nele; Van Bever, Elien; Archer, John R H; Wood, David M; Dargan, Paul I; Van Bortel, Luc; Lambert, Willy E; Stove, Christophe P

    2016-09-23

    Dried blood spot (DBS) sampling and analysis is increasingly being applied in bioanalysis. Although the use of DBS has many advantages, it is also associated with some challenges. E.g. given the limited amount of available material, highly sensitive detection techniques are often required to attain sufficient sensitivity. In gas chromatography coupled to mass spectrometry (GC-MS), derivatization can be helpful to achieve adequate sensitivity. Because this additional sample preparation step is considered as time-consuming, we introduce a new derivatization procedure, i.e. "microwave-assisted on-spot derivatization", to minimize sample preparation of DBS. In this approach the derivatization reagents are directly applied onto the DBS and derivatization takes place in a microwave instead of via conventional heating. In this manuscript we evaluated the applicability of this new concept of derivatization for the determination of two polar low molecular weight molecules, gamma-hydroxybutyric acid (GHB) and gabapentin, in DBS using a standard GC-MS configuration. The method was successfully validated for both compounds, with imprecision and bias values within acceptance criteria (<20% at LLOQ, <15% at 3 other QC levels). Calibration lines were linear over the 10-100μg/mL and 1-30μg/mL range for GHB and gabapentin, respectively. Stability studies revealed no significant decrease of gabapentin and GHB in DBS upon storage at room temperature for at least 84 days. Furthermore, DBS-specific parameters, including hematocrit and volume spotted, were evaluated. As demonstrated by the analysis of GHB and gabapentin positive samples, "microwave-assisted on-spot derivatization" proved to be reliable, fast and applicable in routine toxicology. Moreover, other polar low molecular weight compounds of interest in clinical and/or forensic toxicology, including vigabatrin, beta-hydroxybutyric acid, propylene glycol, diethylene glycol, 1,4-butanediol and 1,2-butanediol, can also be

  5. 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

  6. Identification and quantification of gingerols and related compounds in ginger dietary supplements using high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Tao, Yi; Li, Wenkui; Liang, Wenzhong; Van Breemen, Richard B

    2009-11-11

    Dietary supplements containing preparations of ginger roots/rhizomes (Zingiber officinale Roscoe) are being used by consumers, and clinical trials using ginger dietary supplements have been carried out to evaluate their anti-inflammatory or antiemetic properties with inconsistent results. Chemical standardization of these products is needed for quality control and to facilitate the design of clinical trials and the evaluation of data from these studies. To address this issue, methods based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) were developed for the detection, characterization, and quantitative analysis of gingerol-related compounds in botanical dietary supplements containing ginger roots/rhizomes. During negative ion electrospray with collision-induced dissociation, the cleavage of the C4-C5 bond with a neutral loss of 194 u and benzylic cleavage leading to the neutral loss of 136 u were found to be class-characteristic fragmentation patterns of the pharmacologically active gingerols or shogaols, respectively. On the basis of these results, an assay using LC-MS/MS with neutral loss scanning (loss of 194 or 136 u) was developed that is suitable for the fingerprinting of ginger dietary supplements based on the selective detection of gingerols, shogaols, paradols, and gingerdiones. In addition, a quantitative assay based on LC-MS/MS with selected reaction monitoring was developed for the quantitative analysis of 6-gingerol, 8-gingerol, 10-gingerol, 6-shogaol, 8-shogaol, and 10-shogaol in ginger dietary supplements. After method validation, the quantities of these compounds in three commercially available ginger dietary supplements were determined. This assay showed excellent sensitivity, accuracy, and precision and may be used to address the need for quality control and standardization of ginger dietary supplements. PMID:19817455

  7. 气相色谱-质谱联用分析倍花中化学成分%Compounds Analysis in Beihua by Gas Chromatography-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    欧阳玉祝; 张辞海; 魏燕; 吴道宏

    2013-01-01

    Volatile oils and extracts were prepared from beihua.Compounds in volatile oil and fatty acids in extrats were analyzed by gas chromatography-mass spectrometry.The results showed that fifty compounds were detected from volatile oil with 17.94% of ethyl isopropyl ether,4.4% of hexanoic acid,3.43% of N,N-dimethylaniline,3.72% of dodecanoic acid,14.89% of tetradecanoic acid,8.88% of palmitic acid and 23.8% of cis,cis,cis-7,10,13-hexadecatrienal being the main components.Eighteen compounds were detected from extracts of methyl-esterification,and ten of them are fatty acids.The content of unsaturated fatty acids is 19.2% with linolenic acid being 16.13%,and that of saturated fatty acids is 51.7% with tetradecanoic acid and palmitic acid of 26.88% and 17.03%,respectively.%以植物倍花为原料制备倍花挥发油和倍花提取液,用气相色谱-质谱联用技术分析了挥发油的化学成分和提取液的脂肪酸组成与含量.实验结果表明,挥发油中共检出五十个组分,主要成分是乙基异丙醚、己酸、N,N-二甲基苯胺、月桂酸、肉豆蔻酸、棕榈酸、7(Z),10(Z),13 (Z)-十六碳三烯酮,其相对含量分别为17.94%、4.48%、3.43%、3.72%、14.89%、8.88%、23.8%.倍花提取液经甲酯化后共检出十八种物质,其中有十种脂肪酸,不饱和脂肪酸与饱和脂肪酸总含量分别为19.2%和51.7%;不饱和脂肪酸中亚麻酸含量达16.13%,饱和脂肪酸主要是肉豆蔻酸和棕榈酸,含量分别为26.88%和17.03%.

  8. 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.

  9. 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…

  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. 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

  12. 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.

  13. 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

  14. Selective extraction of halogenated compounds from data measured by comprehensive multidimensional gas chromatography/high resolution time-of-flight mass spectrometry for non-target analysis of environmental and biological samples.

    Science.gov (United States)

    Hashimoto, Shunji; Zushi, Yasuyuki; Fushimi, Akihiro; Takazawa, Yoshikatsu; Tanabe, Kiyoshi; Shibata, Yasuyuki

    2013-03-22

    We developed a method that selectively extracts a subset from comprehensive 2D gas chromatography (GC×GC) and high-resolution time-of-flight mass spectrometry (HRTOFMS) data to detect and identify trace levels of organohalogens. The data were obtained by measuring several environmental and biological samples, namely fly ash, soil, sediment, the atmosphere, and human urine. For global analysis, some samples were measured without purification. By using our novel software, the mass spectra of organochlorines or organobromines were then extracted into a data subset under high mass accuracy conditions that were approximately equivalent to a mass resolution of 6000 for some samples. Mass defect filtering as pre-screening for the data extraction was very effective in removing the mass spectra of hydrocarbons. Those results showed that data obtained with HRTOFMS are valuable for global analysis of organohalogens, and probably of other compounds if specific data extraction methods can be devised.

  15. 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

  16. Development of liquid chromatography-tandem mass spectrometry method for analysis of polyphenolic compounds in liquid samples of grape juice, green tea and coffee.

    Science.gov (United States)

    Sapozhnikova, Yelena

    2014-05-01

    A simple and fast method for the analysis of a wide range of polyphenolic compounds in juice, tea, and coffee samples was developed using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The method was based on a simple sample preparation "dilute and shoot" approach, and LC-MS/MS quantification using genistein-d4 as an internal standard. The performance of six different syringeless filter devices was tested for sample preparation. The method was evaluated for recoveries of polyphenols at three spiking levels in juice, tea, and coffee samples. The recoveries of the majority of polyphenols were satisfactory (70-120%), but some varied significantly (20-138%) depending on the matrix. NIST Standard Reference Materials (SRM) 3257 Catechin Calibration Solutions and 3255 Camellia sinensis (Green Tea) Extract with certified concentrations of catechin and epicatechin were used for method validation. The measurement accuracy in two SRMs was 71-113%. The method was successfully applied to the analysis of liquid samples of grape juice, green tea, and coffee.

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

    Institute of Scientific and Technical Information of China (English)

    Rajasekar Thirunavukkarasu; Priyadharshini Pandiyan; Kumaran Subaramaniyan; Deivasigamani Balaraman; Sakthivel Manikkam; Balamurugan Sadaiyappan; George Edward Gnana Jothi

    2014-01-01

    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.

  19. 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

  20. 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.)

  1. 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

  2. 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

  3. Composition-dependent charge transport and temperature-dependent density of state effective mass interpreted by temperature-normalized Pisarenko plot in Bi2-xSbxTe3 compounds

    Science.gov (United States)

    An, Tae-Ho; Lim, Young Soo; Park, Mi Jin; Tak, Jang-Yeul; Lee, Soonil; Cho, Hyung Koun; Cho, Jun-Young; Park, Chan; Seo, Won-Seon

    2016-10-01

    Composition-dependent charge transport and temperature-dependent density of state effective mass-dependent Seebeck coefficient were investigated in Bi2-xSbxTe3 (x = 1.56-1.68) compounds. The compounds were prepared by the spark plasma sintering of high-energy ball-milled powder. High-temperature Hall measurements revealed that the charge transport in the compounds was governed dominantly by phonon scattering and influenced additionally by alloy scattering depending on the amount of Sb. Contrary effects of Sb content on the Seebeck coefficient were discussed in terms of carrier concentration and density of state effective mass, and it was elucidated by temperature-normalized Pisarenko plot for the first time.

  4. Iodine neutron capture therapy

    Science.gov (United States)

    Ahmed, Kazi Fariduddin

    A new technique, Iodine Neutron Capture Therapy (INCT) is proposed to treat hyperthyroidism in people. Present thyroid therapies, surgical removal and 131I treatment, result in hypothyroidism and, for 131I, involve protracted treatment times and excessive whole-body radiation doses. The new technique involves using a low energy neutron beam to convert a fraction of the natural iodine stored in the thyroid to radioactive 128I, which has a 24-minute half-life and decays by emitting 2.12-MeV beta particles. The beta particles are absorbed in and damage some thyroid tissue cells and consequently reduce the production and release of thyroid hormones to the blood stream. Treatment times and whole-body radiation doses are thus reduced substantially. This dissertation addresses the first of the several steps needed to obtain medical profession acceptance and regulatory approval to implement this therapy. As with other such programs, initial feasibility is established by performing experiments on suitable small mammals. Laboratory rats were used and their thyroids were exposed to the beta particles coming from small encapsulated amounts of 128I. Masses of 89.0 mg reagent-grade elemental iodine crystals have been activated in the ISU AGN-201 reactor to provide 0.033 mBq of 128I. This activity delivers 0.2 Gy to the thyroid gland of 300-g male rats having fresh thyroid tissue masses of ˜20 mg. Larger iodine masses are used to provide greater doses. The activated iodine is encapsulated to form a thin (0.16 cm 2/mg) patch that is then applied directly to the surgically exposed thyroid of an anesthetized rat. Direct neutron irradiation of a rat's thyroid was not possible due to its small size. Direct in-vivo exposure of the thyroid of the rat to the emitted radiation from 128I is allowed to continue for 2.5 hours (6 half-lives). Pre- and post-exposure blood samples are taken to quantify thyroid hormone levels. The serum T4 concentration is measured by radioimmunoassay at

  5. 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...

  6. 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

  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. 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.

  9. Identification of non-volatile compounds and their migration from hot melt adhesives used in food packaging materials characterized by ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Vera, Paula; Canellas, Elena; Nerín, Cristina

    2013-05-01

    The identification of unknown non-volatile migrant compounds from adhesives used in food contact materials is a very challenging task because of the number of possible compounds involved, given that adhesives are complex mixtures of chemicals. The use of ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UPLC-MS/QTOF) is shown to be a successful tool for identifying non-targeted migrant compounds from two hot melt adhesives used in food packaging laminates. Out of the seven migrants identified and quantified, five were amides and one was a compound classified in Class II of the Cramer toxicity. None of the migration values exceeded the recommended Cramer exposure values.

  10. 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.

  11. Capture ready study

    Energy Technology Data Exchange (ETDEWEB)

    Minchener, A.

    2007-07-15

    There are a large number of ways in which the capture of carbon as carbon dioxide (CO{sub 2}) can be integrated into fossil fuel power stations, most being applicable for both gas and coal feedstocks. To add to the choice of technology is the question of whether an existing plant should be retrofitted for capture, or whether it is more attractive to build totally new. This miscellany of choices adds considerably to the commercial risk of investing in a large power station. An intermediate stage between the non-capture and full capture state would be advantageous in helping to determine the best way forward and hence reduce those risks. In recent years the term 'carbon capture ready' or 'capture ready' has been coined to describe such an intermediate stage plant and is now widely used. However a detailed and all-encompassing definition of this term has never been published. All fossil fuel consuming plant produce a carbon dioxide gas byproduct. There is a possibility of scrubbing it with an appropriate CO{sub 2} solvent. Hence it could be said that all fossil fuel plant is in a condition for removal of its CO{sub 2} effluent and therefore already in a 'capture ready' state. Evidently, the practical reality of solvent scrubbing could cost more than the rewards offered by such as the ETS (European Trading Scheme). In which case, it can be said that although the possibility exists of capturing CO{sub 2}, it is not a commercially viable option and therefore the plant could not be described as ready for CO{sub 2} capture. The boundary between a capture ready and a non-capture ready condition using this definition cannot be determined in an objective and therefore universally acceptable way and criteria must be found which are less onerous and less potentially contentious to assess. 16 refs., 2 annexes.

  12. 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.

  13. 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.

  14. Characterization of sulfur compounds in whisky by full evaporation dynamic headspace and selectable one-dimensional/two-dimensional retention time locked gas chromatography-mass spectrometry with simultaneous element-specific detection.

    Science.gov (United States)

    Ochiai, Nobuo; Sasamoto, Kikuo; MacNamara, Kevin

    2012-12-28

    A method is described for characterization of sulfur compounds in unaged and aged whisky. The method is based on full evaporation dynamic headspace (FEDHS) of 100 μL of whisky samples followed by selectable one-dimensional ((1)D) or two-dimensional ((2)D) retention-time-locked (RTL) gas chromatography (GC)-mass spectrometry (MS) with simultaneous element-specific detection using a sulfur chemiluminescence detector (SCD) and a nitrogen chemiluminescence detector (NCD). Sequential heart-cuts of the 16 sulfur fractions were used to identify each individual sulfur compound in the unaged whisky. Twenty sulfur compounds were positively identified by a MS library search, linear retention indices (LRI), and formula identification using MS calibration software. Additionally eight formulas were also identified for unknown sulfur compounds. Simultaneous heart-cuts of the 16 sulfur fractions were used to produce the (2)D RTL GC-SCD chromatograms for principal component analysis. PCA of the (2)D RTL GC-SCD data clearly demonstrated the difference between unaged and aged whisky, as well as two different whisky samples. Fourteen sulfur compounds could be characterized as key sulfur compounds responsible for the changes in the aging step and/or the difference between two kinds of whisky samples. The determined values of the key sulfur compounds were in the range of 0.3-210 ng mL(-1) (RSD: 0.37-12%, n=3).

  15. Application of dispersive liquid-liquid microextraction and gas chromatography with mass spectrometry for the determination of oxygenated volatile organic compounds in effluents from the production of petroleum bitumen.

    Science.gov (United States)

    Boczkaj, Grzegorz; Makoś, Patrycja; Przyjazny, Andrzej

    2016-07-01

    We present a new procedure for the determination of oxygenated volatile organic compounds in samples of postoxidative effluents from the production of petroleum bitumens using dispersive liquid-liquid microextraction and gas chromatography with mass spectrometry. The eight extraction parameters were optimized for 43 oxygenated volatile organic compounds. The detection limits obtained ranged from 0.07 to 0.82 μg/mL for most of the analytes, the precision was good (relative standard deviation below 2.91% at the 5 μg/mL level and 4.75% at the limit of quantification), the recoveries for the majority of compounds varied from 70.6 to 118.9%, and the linear range was wide, which demonstrates the usefulness of the procedure. The developed procedure was used for the determination of oxygenated volatile organic compounds in samples of raw postoxidative effluents and in effluents after chemical treatment. In total, 23 compounds at concentration levels from 0.37 to 32.95 μg/mL were identified in real samples. The same samples were also analyzed in the SCAN mode, which resulted in four more phenol derivatives being identified and tentatively determined. The studies demonstrated the need for monitoring volatile organic compounds content in effluents following various treatments due to the formation of secondary oxygenated volatile organic compounds.

  16. Determination of estrogenic compounds in milk and yogurt samples by hollow-fibre liquid-phase microextraction-gas chromatography-triple quadrupole mass spectrometry.

    Science.gov (United States)

    D'Orazio, Giovanni; Hernández-Borges, Javier; Herrera-Herrera, Antonio Vicente; Fanali, Salvatore; Rodríguez-Delgado, Miguel Ángel

    2016-10-01

    An environmentally friendly method based on hollow-fibre liquid-phase microextraction (HF-LPME) was developed for the extraction of selected estrogenic compounds (i.e. four natural sexual hormones: estrone, 17β-estradiol, 17α-estradiol and estriol; two exoestrogens: 17α-ethynylestradiol and 2-methoxyestradiol; two synthetic stilbenes: dienestrol and hexestrol; and five resorcylic acid lactones: zearalenone, α-zearalanol, β-zearalanol, α-zearalenol and β-zearalenol), from whole cow and semi-skimmed goat milk and whole natural yogurt. After the optimization of the sample preparation procedure, spiked extracts were derivatized to their trimethylsilyl products using N,O-bis(trimethylsilyl)trifluoroacetamide reagent and then analyzed by gas chromatography-tandem mass spectrometry (GC-MS/MS). Once optimum extraction conditions were established (protein precipitation with acetonitrile, extraction and the back-extraction in acetonitrile following the HF-LPME procedure), the method was validated and the calibration range, precision and accuracy were studied. The RSD values for the intra- and inter-day precision of the peak areas were in the range 0.65-9.69 and 1.00-11.47 %, respectively. The determination coefficients were higher than 0.991 for method calibration curves while LOD and LOQ values were between 0.06-2.55 and 0.16-6.11 μg/L for whole cow milk, 0.04-1.70 and 0.11-4.86 μg/L for semi-skimmed goat milk and 0.07-3.73 and 0.23-9.81 μg/L for natural yogurt, respectively. Finally, the accuracy and precision of the method were evaluated, obtaining a value in the range 84 81-119 % and RSD values lower than 20 % in all cases.

  17. 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.

  18. Determination of estrogenic compounds in milk and yogurt samples by hollow-fibre liquid-phase microextraction-gas chromatography-triple quadrupole mass spectrometry.

    Science.gov (United States)

    D'Orazio, Giovanni; Hernández-Borges, Javier; Herrera-Herrera, Antonio Vicente; Fanali, Salvatore; Rodríguez-Delgado, Miguel Ángel

    2016-10-01

    An environmentally friendly method based on hollow-fibre liquid-phase microextraction (HF-LPME) was developed for the extraction of selected estrogenic compounds (i.e. four natural sexual hormones: estrone, 17β-estradiol, 17α-estradiol and estriol; two exoestrogens: 17α-ethynylestradiol and 2-methoxyestradiol; two synthetic stilbenes: dienestrol and hexestrol; and five resorcylic acid lactones: zearalenone, α-zearalanol, β-zearalanol, α-zearalenol and β-zearalenol), from whole cow and semi-skimmed goat milk and whole natural yogurt. After the optimization of the sample preparation procedure, spiked extracts were derivatized to their trimethylsilyl products using N,O-bis(trimethylsilyl)trifluoroacetamide reagent and then analyzed by gas chromatography-tandem mass spectrometry (GC-MS/MS). Once optimum extraction conditions were established (protein precipitation with acetonitrile, extraction and the back-extraction in acetonitrile following the HF-LPME procedure), the method was validated and the calibration range, precision and accuracy were studied. The RSD values for the intra- and inter-day precision of the peak areas were in the range 0.65-9.69 and 1.00-11.47 %, respectively. The determination coefficients were higher than 0.991 for method calibration curves while LOD and LOQ values were between 0.06-2.55 and 0.16-6.11 μg/L for whole cow milk, 0.04-1.70 and 0.11-4.86 μg/L for semi-skimmed goat milk and 0.07-3.73 and 0.23-9.81 μg/L for natural yogurt, respectively. Finally, the accuracy and precision of the method were evaluated, obtaining a value in the range 84 81-119 % and RSD values lower than 20 % in all cases. PMID:27526090

  19. 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

  20. CAPTURED Ghana Country Evaluation

    NARCIS (Netherlands)

    Sefa Dei, G.J.; Brouwers, J.H.A.M.

    2012-01-01

    This report provides the findings of the Ghana Country Evaluation and is produced as part of the overall CAPTURED End Evaluation. After five years of support by the CAPTURED project the University of Development Studies has been able to achieve commendable results. It can be confirmed that the conte

  1. 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

  2. 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

  3. 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.

  4. Resonance-enhanced multiphoton ionization time-of-flight mass spectrometry for detection of nitrogen containing aliphatic and aromatic compounds: resonance-enhanced multiphoton ionization spectroscopic investigation and on-line analytical application.

    Science.gov (United States)

    Streibel, T; Hafner, K; Mühlberger, F; Adam, T; Zimmermann, R

    2006-01-01

    Resonance-enhanced multiphoton ionization (REMPI) combined with time-of-flight mass spectrometry (TOFMS) is an analytical method capable of on-line monitoring of trace compounds in complex matrices. A necessary prerequisite for substance selective detection is spectroscopic investigation of the target molecules. Several organic nitrogen compounds comprising aliphatic and aromatic amines, nitrogen heterocyclic compounds, and aromatic nitriles are spectroscopically investigated with a tunable narrow bandwidth optical parametric oscillator (OPO) laser system providing a scannable wavelength range between 220 and 340 nm. These species are known as possible precursors in fuel-NO formation from combustion of solid fuels such as biomass and waste. A newly conceived double inlet system was used in this study, which allows rapid change between effusive and supersonic molecular beams. The resulting REMPI spectra of the compounds are discussed with respect to electronic transitions that could be utilized for a selective ionization of these compounds in complex mixtures such as combustion and process gases. The practicability of this approach is demonstrated by wavelength selected on-line REMPI-TOFMS detection of aniline and cyanonaphthalene in the burning chamber of a waste incineration plant. REMPI mass spectra recorded at different excitation wavelengths as well as variations in time show the utilization of species-selective REMPI-TOFMS detection for on-line monitoring of crucial substances in pollutant formation.

  5. 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.

  6. 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

  7. 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

  8. 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...

  9. 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.

  10. 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

  11. Determination of butyl- and phenyltin compounds in human urine by HS-SPME after derivatization with tetraethylborate and subsequent determination by capillary GC with microwave-induced plasma atomic emission and mass spectrometric detection.

    Science.gov (United States)

    Zachariadis, G A; Rosenberg, E

    2009-04-30

    A headspace solid-phase micro-extraction (HS-SPME) method was developed and optimized for gas chromatographic separation and determination of commonly found organotin compounds in human urine after potential exposure. Butyl- and phenyltin compounds were in situ derivatized to ethylated derivatives by sodium tetraethylborate (NaBEt(4)) directly in the urine matrix. The relevant parameters affecting the yield of the SPME procedure were examined using tetrabutyltin as internal standard. The method was optimized for direct use in the analysis of undiluted human urine samples and mono-, di- and tri-substituted butyl- and phenyltin compounds could be determined after a 15-min headspace extraction time at room temperature. The selectivity of the microwave-induced plasma atomic emission detector (MIP-AED) as an element specific detector in combination with the relatively selective sample preparation technique of HS-SPME allowed the interference-free detection of the organotin compounds in all cases. A quadrupole mass spectrometer was used in parallel experiments as a detector for the confirmation of the identity molecular structure of the eluted compounds. The performance characteristics of the developed method are given for the determination of mixtures of these compounds. Finally the proposed method was applied to the analysis of several human urine samples. PMID:19203626

  12. 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

  13. 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

  14. Marine turtle capture data

    Data.gov (United States)

    National Oceanic and Atmospheric Administration, Department of Commerce — To estimate abundance, growth, and survival rate and to collect tissue samples, marine turtles are captured at nesting beaches and foraging grounds through various...

  15. 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

  16. 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.

  17. 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...

  18. 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...

  19. 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...

  20. 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

  1. 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

  2. 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.

  3. 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.

  4. 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.

  5. 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

  6. 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.

  7. 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

  8. 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.

  9. 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

  10. 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

  11. 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...

  12. 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.

  13. 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

  14. Proton capture resonance studies

    Energy Technology Data Exchange (ETDEWEB)

    Mitchell, G.E. [North Carolina State University, Raleigh, North Carolina (United States) 27695]|[Triangle Universities Nuclear Laboratory, Durham, North Carolina (United States) 27708; Bilpuch, E.G. [Duke University, Durham, North Carolina (United States) 27708]|[Triangle Universities Nuclear Laboratory, Durham, North Carolina (United States) 27708; Bybee, C.R. [North Carolina State University, Raleigh, North Carolina (United States) 27695]|[Triangle Universities Nuclear Laboratory, Durham, North Carolina (United States) 27708; Cox, J.M.; Fittje, L.M. [Tennessee Technological University, Cookeville, Tennessee (United States) 38505]|[Triangle Universities Nuclear Laboratory, Durham, North Carolina (United States) 27708; Labonte, M.A.; Moore, E.F.; Shriner, J.D. [North Carolina State University, Raleigh, North Carolina (United States) 27695]|[Triangle Universities Nuclear Laboratory, Durham, North Carolina (United States) 27708; Shriner, J.F. Jr. [Tennessee Technological University, Cookeville, Tennessee (United States) 38505]|[Triangle Universities Nuclear Laboratory, Durham, North Carolina (United States) 27708; Vavrina, G.A. [North Carolina State University, Raleigh, North Carolina (United States) 27695]|[Triangle Universities Nuclear Laboratory, Durham, North Carolina (United States) 27708; Wallace, P.M. [Duke University, Durham, North Carolina (United States) 27708]|[Triangle Universities Nuclear Laboratory, Durham, North Carolina (United States) 27708

    1997-02-01

    The fluctuation properties of quantum systems now are used as a signature of quantum chaos. The analyses require data of extremely high quality. The {sup 29}Si(p,{gamma}) reaction is being used to establish a complete level scheme of {sup 30}P to study chaos and isospin breaking in this nuclide. Determination of the angular momentum J, the parity {pi}, and the isospin T from resonance capture data is considered. Special emphasis is placed on the capture angular distributions and on a geometric description of these angular distributions. {copyright} {ital 1997 American Institute of Physics.}

  15. 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.

  16. 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.

  17. 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

  18. 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

  19. 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

  20. 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

  1. Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory - Determination of Wastewater Compounds by Polystyrene-Divinylbenzene Solid-Phase Extraction and Capillary-Column Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Zaugg, Steven D.; Smith, Steven G.; Schroeder, Michael P.; Barber, Larry B.; Burkhardt, Mark R.

    2002-01-01

    A method for the determination of 67 compounds typically found in domestic and industrial wastewater is described. The method was developed in response to increasing concern over the impact of endocrine-disrupting chemicals in wastewater on aquatic organisms. This method also may be useful for evaluating the impact of combined sanitary and storm-sewer overflow on the water quality of urban streams. The method focuses on the determination of compounds that are an indicator of wastewater or that have been 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, polycyclicaromatic hydrocarbons, and high-use domestic pesticides. Water samples are filtered to remove suspended particulate matter and then are extracted by vacuum through disposable solid-phase cartridges that contain polystyrene-divinylbenzene resin. Cartridges are dried with nitrogen gas, and then sorbed compounds are eluted with dichloromethane-diethyl ether (4:1) and determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-water samples fortified at 4 micrograms per liter averaged 74 percent ? 7 percent relative standard deviation for all method compounds. Initial method detection limits for single-component compounds (excluding hormones and sterols) averaged 0.15 microgram per liter. Samples are preserved by filtration, the addition of 60 grams NaCl, and storage at 4 degrees Celsius. The laboratory has established a sample-holding time (prior to sample extraction) of 14 days from the date of sample collection until a statistically accepted method can be used to determine the effectiveness of these sample-preservation procedures.

  2. 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.

  3. 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.

  4. 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...

  5. 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.

  6. Mass of chlorinated volatile organic compounds removed by Pump-and-Treat, Naval Air Warfare Center, West Trenton, New Jersey, 1996-2010

    Science.gov (United States)

    Lacombe, Pierre J.

    2011-01-01

    Pump and Treat (P&T) remediation is the primary technique used to contain and remove trichloroethylene (TCE) and its degradation products cis 1-2,dichloroethylene (cDCE) and vinyl chloride (VC) from groundwater at the Naval Air Warfare Center (NAWC), West Trenton, NJ. Three methods were used to determine the masses of TCE, cDCE, and VC removed from groundwater by the P&T system since it became fully operational in 1996. Method 1, is based on the flow volume and concentrations of TCE, cDCE, and VC in groundwater that entered the P&T building as influent. Method 2 is based on withdrawal volume from each active recovery well and the concentrations of TCE, cDCE, and VC in the water samples from each well. Method 3 compares the maximum monthly amount of TCE, cDCE, and VC from Method 1 and Method 2. The greater of the two values is selected to represent the masses of TCE, cDCE and VC removed from groundwater each month. Previously published P&T monthly reports used Method 1 to determine the mass of TCE, cDCE, and VC removed. The reports state that 8,666 pounds (lbs) of TCE, 13,689 lbs of cDCE, and 2,455 lbs of VC were removed by the P&T system during 1996-2010. By using Method 2, the mass removed was determined to be 8,985 lbs of TCE, 17,801 lbs of cDCE, and 3,056 lbs of VC removed, and Method 3, resulted in 10,602 lbs of TCE, 21,029 lbs of cDCE, and 3,496 lbs of VC removed. To determine the mass of original TCE removed from groundwater, the individual masses of TCE, cDCE, and VC (determined using Methods 1, 2, and 3) were converted to numbers of moles, summed, and converted to pounds of original TCE. By using the molar conversion the mass of original TCE removed from groundwater by Methods 1, 2, and 3 was 32,381 lbs, 39,535 lbs, and 46,452 lbs, respectively, during 1996-2010. P&T monthly reports state that 24,805 lbs of summed TCE, cDCE, and VC were removed from groundwater. The simple summing method underestimates the mass of original TCE removed by the P&T system.

  7. Neutron capture by hook or by crook

    Science.gov (United States)

    Mosby, Shea

    2016-03-01

    The neutron capture reaction is a topic of fundamental interest for both heavy element (A>60) nucleosynthesis and applications in such fields as nuclear energy and defense. The full suite of interesting isotopes ranges from stable nuclei to the most exotic, and it is not possible to directly measure all the relevant reaction rates. The DANCE instrument at Los Alamos provides direct access to the neutron capture reaction for stable and long-lived nuclei, while Apollo coupled to HELIOS at Argonne has been developed as an indirect probe for cases where a direct measurement is impossible. The basic techniques and their implications will be presented, and the status of ongoing experimental campaigns to address neutron capture in the A=60 and A=100 mass regions will be discussed.

  8. Muon capture rates within the projected QRPA

    CERN Document Server

    Santos, Danilo Sande; Krmpotić, Francisco; Dimarco, Alejandro J

    2012-01-01

    The conservation of the number of particles within the QRPA plays an important role in the evaluation muon capture rates in all light nuclei with A \\precsim 30 . The violation of the CVC by the Coulomb field in this mass region is of minor importance, but this effect could be quite relevant for medium and heavy nuclei studied previously. The extreme sensitivity of the muon capture rates on the 'pp' coupling strength in nuclei with large neutron excess when described within the QRPA is pointed out. We reckon that the comparison between theory and data for the inclusive muon capture is not a fully satisfactory test on the nuclear model that is used. The exclusive muon transitions are much more robust for such a purpose.

  9. Laser capture microscopy

    OpenAIRE

    Curran, S.; McKay, J A; McLeod, H L; Murray, G I

    2000-01-01

    Human tissues are composed of complex admixtures of different cell types and their biologically meaningful analysis necessitates the procurement of pure samples of the cells of interest. Many approaches have been used in attempts to overcome this difficulty, including a variety of microdissection methods. This review concerns a recent advance in microdissection techniques, namely laser capture microdissection (LCM). The principle underlying this technique is outlined, and practical issues per...

  10. Supernova electron capture rates

    CERN Document Server

    Martínez-Pinedo, G

    1999-01-01

    We have calculated the Gamow-Teller strength distributions for the ground states and low lying states of several nuclei that play an important role in the precollapse evolution of supernova. The calculations reproduce the experimental GT distributions nicely. The GT distribution are used to calculate electron capture rates for typical presupernova conditions. The computed rates are noticeably smaller than the presently adopted rates. The possible implications for the supernova evolution are discussed.

  11. Experimental assessment and modeling of interphase mass transfer rates of organic compounds in multiphase subsurface systems. Final report, July 1, 1989--June 30, 1993

    Energy Technology Data Exchange (ETDEWEB)

    Abriola, L.M.; Weber, W.J. Jr.

    1993-10-01

    Results of an experimental investigation into strady state dissolution of nonaqueous phase liquids (NAPLS) entrapped within water saturated porous media are presented. Influence of porous media type, NAPL characteristics, and aqueous phase flow velocity are examined for transient and steady-state dissolution of NAPL. Entrapped NAPL distributions are examined and are found to influence mass transfer between the phases. A phenomenological model for the steady state mass transfer process is developed which expresses a lumped mass transfer coefficient as a function of the hydrodynamics of the system and grain size parameters as a surrogate measure of the NAPL distribution. Transient dissolution data is used to develop two alternative phenomenological models for mass transfer. The models are incorporated into a onedimensional numerical simulator and are shown to be effective predictors of transient dissolution data in similar experimental systems. In order to further explore the effects of scale and heterogeneities on NAPL dissolution, the sphere model is incorporated into a two-dimensional simulator and is used to explore long-term dissolution of a TCE (trichloroethylene) spill in a layered system of sands. The simulation demonstrates the significance of heterogeneity, both in controlling the initial distribution of NAPL and the rate of NAPL dissolution.

  12. A microwave-mediated saponification of galactosylceramide and galactosylceramide I3-sulfate and identification of their lyso-compounds by delayed extraction matrix-assisted laser desorption ionization time-of-flight mass spectrometry.

    Science.gov (United States)

    Taketomi, T; Hara, A; Uemura, K; Kurahashi, H; Sugiyama, E

    1996-07-16

    Small amounts of galactosylceramide (cerebroside) and galactosylceramide I3-sulfate (sulfatide) obtained from porcine spinal cord and equine kidney were deacylated by a rapid method of microwave-mediated saponification to prepare their lyso-compounds. Mass spectra of their protonated or deprotonated molecular ion peaks were detected by recently developed new technology of a delayed extraction matrix-assisted laser desorption ionization time-of-flight mass spectrometer with reflector detector in positive or negative ion mode. Long chain bases of lysocerebroside and lysosulfatide were different between porcine spinal cord and equine kidney, but similar to each other in the same organ, suggesting their common synthetic pathway. It is noted that the new rapid method can be similarly applied to the deacylation of both cerebroside and sulfatide in contrast to our classical method which was able to be applied to cerebroside, but not to sulfatide.

  13. Technology Roadmap: Carbon Capture and Storage

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2013-08-01

    As long as fossil fuels and carbon-intensive industries play dominant roles in our economies, carbon capture and storage (CCS) will remain a critical greenhouse gas reduction solution. This CCS roadmap aims at assisting governments and industry in integrating CCS in their emissions reduction strategies and in creating the conditions for scaled-up deployment of all three components of the CCS chain: CO2 capture, transport and storage. To get us onto the right pathway, this roadmap highlights seven key actions needed in the next seven years to create a solid foundation for deployment of CCS starting by 2020. IEA analysis shows that CCS is an integral part of any lowest-cost mitigation scenario where long-term global average temperature increases are limited to significantly less than 4 °C, particularly for 2 °C scenarios (2DS). In the 2DS, CCS is widely deployed in both power generation and industrial applications. The total CO2 capture and storage rate must grow from the tens of megatonnes of CO2 captured in 2013 to thousands of megatonnes of CO2 in 2050 in order to address the emissions reduction challenge. A total cumulative mass of approximately 120 GtCO2 would need to be captured and stored between 2015 and 2050, across all regions of the globe.

  14. Identification of active compounds and their metabolites by high-performance liquid chromatography/electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry from Xiao-xu-ming decoction (XXMD).

    Science.gov (United States)

    Wang, Yilin; Ding, Chunguang; Du, Kehe; Xiao, Yao; Wu, Caisheng; Zhang, Jinlan; Qin, Hailin; Du, Guanhua

    2009-09-01

    Xiao-xu-ming decoction (XXMD) prescription is a traditional Chinese prescription that has been widely used to treat theoplegia and the sequela of theoplegia. Modern pharmacological research has also indicated that the active fraction from XXMD is able to treat cardiovascular diseases and Alzheimer's disease. In the study reported here, high-performance liquid chromatography coupled with Fourier transform ion cyclotron resonance mass spectrometry (HPLC/FTICR-MS) was developed to identify active compounds and their metabolites after oral administration of active fraction from Xiao-xu-ming decoction to rats, using parent mass list triggered data-dependent multiple-stage mass analysis at a resolving power of 100,000 in the external calibration mode. The mass accuracies obtained for full-scan MS were within 2 ppm in most cases. Fifteen constituents were identified in the active fraction from XXMD and the biological samples of rats. The fragmentation behaviors of these constituents were summarized which would be helpful for structural characterization. The profiles of the constituents in the active fraction and biological samples of rats were obtained which provided us with much information for a better understanding of the chemical basis of the pharmacologic actions of XXMD.

  15. Rapid fingerprinting of sterols and related compounds in vegetable and animal oils and phytosterol enriched- margarines by transmission mode direct analysis in real time mass spectrometry.

    Science.gov (United States)

    Alberici, Rosana M; Fernandes, Gabriel D; Porcari, Andréia M; Eberlin, Marcos N; Barrera-Arellano, Daniel; Fernández, Facundo M

    2016-11-15

    Plant-derived sterols, often referred to as phytosterols, are important constituents of plant membranes where they assist in maintaining phospholipid bilayer stability. Consumption of phytosterols has been suggested to positively affect human health by reducing cholesterol levels in blood via inhibition of its absorption in the small intestine, thus protecting against heart attack and stroke. Sterols are challenging analytes for mass spectrometry, since their low polarity makes them difficult to ionize by both electrospray ionization (ESI) and matrix-assisted laser desorption ionization (MALDI), typically requiring derivatization steps to overcome their low ionization efficiencies. We present a fast and reliable method to characterize the composition of phytosterols in vegetable oils and enriched margarines. The method requires no derivatization steps or sample extraction procedures thanks to the use of transmission mode direct analysis in real time mass spectrometry (TM-DART-MS). PMID:27283681

  16. Determination of nitrophenolic compounds from atmospheric particles using hollow-fiber liquid-phase microextraction and capillary electrophoresis/mass spectrometry analysis.

    Science.gov (United States)

    Teich, Monique; van Pinxteren, Dominik; Herrmann, Hartmut

    2014-05-01

    A hollow-fiber liquid-phase microextraction method was developed to enrich nine nitrophenolic compounds from aqueous extracts of atmospheric aerosol particles. Analysis was performed by CE coupled with ESI MS. The BGE composition was optimized to a 20 mM ammonium acetate buffer at pH 9.7 containing 15% methanol v/v. Several extraction parameters (composition of organic liquid membrane, pH of acceptor phase, salting-out effect, extraction time) were investigated for their effect on the analyte recoveries. The donor phase consisted of a 1.8 mL sample solution kept at pH 2 while the acceptor phase was a 15 μL 100 mM aqueous ammonia solution. Dihexyl ether served as supported liquid membrane. Low detection limits in the range of nanomole per liter were achieved. Recoveries of aqueous standard solutions were found to be between 11 and 90% with enrichment factors between 10 and 100. Interday and intraday repeatabilities were in an acceptable range for most compounds (6-15% and 7-10%, respectively) but somewhat higher for 4-nitrocatechol (59 and 48%) and 2-nitrophenol (17 and 35%). The developed method was found to be competitive with more established method and was successfully applied to samples of atmospheric particulate matter from field experiments.

  17. Effects of Conventional Heating on the Stability of Major Olive Oil Phenolic Compounds by Tandem Mass Spectrometry and Isotope Dilution Assay

    OpenAIRE

    Giovanni Sindona; Hicham Benabdelkamel; Anna Russo; Enzo Perri; Mohamed Attya

    2010-01-01

    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...

  18. Separation of selenium, zinc, and copper compounds in bovine whey using size exclusion chromatography linked to inductively coupled plasma mass spectrometry.

    OpenAIRE

    Hoac, Tien; Lundh, Thomas; Purup, Stig; Onning, Gunilla; Sejrsen, Kristen; Akesson, Bjorn

    2007-01-01

    To study the role of trace elements for the quality and nutritional value of bovine milk, the distribution of selenium, zinc, and copper in whey was investigated using a method linking size exclusion chromatography to inductively coupled plasma mass spectrometry (SEC-ICP-MS). Three major peaks were detected for selenium, two peaks for zinc, and five peaks for copper. More than 65% of the selenium was found in protein fractions, mainly in fractions coinciding with the major whey proteins beta-...

  19. Changes in color-related compounds in tomato fruit exocarp and mesocarp during ripening using HPLC-APcI+-mass Spectrometry

    OpenAIRE

    Carrillo-López, A.; Yahia, E.M.

    2012-01-01

    Tomato is an important agricultural crop world-wide. Their pigments are very important in many ways. They have been associated with health benefits such as lowering the risk of some chronic diseases. Quantification of chlorophylls by spectrophotometry and Identification of carotenoids using liquid chromatography coupled to mass spectrometry, and quantification by HPLC-DAD was carried out in the exocarp and mesocarp of tomato fruit during 6 different ripeness stages (mature-green, breakers, tu...

  20. Study of mass attenuation coefficients, effective atomic numbers and electron densities for some low Z compounds of dosimetry interest at 59.54 keV incident photon energy

    International Nuclear Information System (INIS)

    Highlights: ► Gamma-ray interaction parameters of some low Z compounds have been measured at 59.54 keV. ► Values of effective atomic numbers (Zeff) have been obtained using an alternative approach based upon interpolation method. ► Composite materials investigated behave as incoherent scatters. ► Selected compounds can be represented by single (valued) mean atomic number 〈Z〉 at incident photon energy. ► Data presented is expected to be useful in medical based applications of nuclear radiation. - Abstract: Total mass attenuation coefficient, total photon interaction cross-section, effective atomic numbers (Zeff) and electron densities (Ne) of Aniline (C6H5NH2), Cyclohexane (C6H12), Glycerine (C3H5(OH)3), Butyl alcohol N-(C4H9OH), DMSO – dimethyl sulfoxide (C2H6OS), Methyl ethyl-ketone (C4H8O), Xylene (C8H10), Acetophenone (C8H8O) and Triethyl amine (C6H15N) have been measured at 59.54 keV energy photon emitted by 100 mCi 241Am point source employing narrow beam transmission geometry. Obtained results have been compared with theoretically calculated values of XCOM (Berger and Hubbel, 1987) and FFAST (). Mixture rule was employed to calculated theoretical mass attenuation coefficient values for each sample. Good agreement has been observed between experimental and theoretical values within experimental uncertainties.

  1. A high-resolution time-of-flight chemical ionization mass spectrometer utilizing hydronium ions (H3O+ ToF-CIMS) for measurements of volatile organic compounds in the atmosphere

    Science.gov (United States)

    Yuan, Bin; Koss, Abigail; Warneke, Carsten; Gilman, Jessica B.; Lerner, Brian M.; Stark, Harald; de Gouw, Joost A.

    2016-07-01

    Proton transfer reactions between hydronium ions (H3O+) and volatile organic compounds (VOCs) provide a fast and highly sensitive technique for VOC measurements, leading to extensive use of proton-transfer-reaction mass spectrometry (PTR-MS) in atmospheric research. Based on the same ionization approach, we describe the development of a high-resolution time-of-flight chemical ionization mass spectrometer (ToF-CIMS) utilizing H3O+ as the reagent ion. The new H3O+ ToF-CIMS has sensitivities of 100-1000 cps ppb-1 (ion counts per second per part-per-billion mixing ratio of VOC) and detection limits of 20-600 ppt at 3σ for a 1 s integration time for simultaneous measurements of many VOC species of atmospheric relevance. The ToF analyzer with mass resolution (m/Δm) of up to 6000 allows the separation of isobaric masses, as shown in previous studies using similar ToF-MS. While radio frequency (RF)-only quadrupole ion guides provide better overall ion transmission than ion lens system, low-mass cutoff of RF-only quadrupole causes H3O+ ions to be transmitted less efficiently than heavier masses, which leads to unusual humidity dependence of reagent ions and difficulty obtaining a humidity-independent parameter for normalization. The humidity dependence of the instrument was characterized for various VOC species and the behaviors for different species can be explained by compound-specific properties that affect the ion chemistry (e.g., proton affinity and dipole moment). The new H3O+ ToF-CIMS was successfully deployed on the NOAA WP-3D research aircraft for the SONGNEX campaign in spring of 2015. The measured mixing ratios of several aromatics from the H3O+ ToF-CIMS agreed within ±10 % with independent gas chromatography measurements from whole air samples. Initial results from the SONGNEX measurements demonstrate that the H3O+ ToF-CIMS data set will be valuable for the identification and characterization of emissions from various sources, investigation of secondary

  2. Fast Detection of Phenolic Compounds in Extracts of Easter Pears (Pyrus communis from the Atacama Desert by Ultrahigh-Performance Liquid Chromatography and Mass Spectrometry (UHPLC–Q/Orbitrap/MS/MS

    Directory of Open Access Journals (Sweden)

    Mario J. Simirgiotis

    2016-01-01

    Full Text Available A small Chilean variety of pears growing in the town of Toconao, an oasis located at the northeastern edge of the Salar de Atacama, northern Chile, was studied by means of modern PDA and high resolution mass spectral data (UHPLC-PDA-HESI-orbitrap-MS/MS. In addition, the antioxidant features of the fruits were compared with the varieties Packhman’s Triumph and Abate Fetel and correlated with the presence of phenolic compounds. The non-pigmented phenolics were fingerprinted and related to the antioxidant capacities measured by the bleaching of the DPPH radical, the ferric reducing antioxidant power (FRAP, the superoxide anion scavenging activity assay (SA, and total content of phenolics and flavonoids measured by spectroscopic methods. The machine allowed a fast separation of 15 min employing a flow rate of 1 mL per minute and could accurately identify 25 compounds, including several isorhamnetin derivatives and phenolic acids, present in the peel and pulps of this Chilean variety for the first time. The compounds were monitored using a wavelength range of 210–800 nm. The native small Chilean pear showed the highest antioxidant activity measured as the bleaching of the DPPH radical, the ferric reducing antioxidant power and superoxide anion scavenging activity (8.61 ± 0.65 μg/mL, 712.63 ± 12.12 micromols trolox equivalents (μmol/TE/100 g FW, and 82.89% ± 2.52% at 100 μg/mL, respectively.

  3. Analysis of volatile organic compounds released from the decay of surrogate human models simulating victims of collapsed buildings by thermal desorption-comprehensive two-dimensional gas chromatography-time of flight mass spectrometry.

    Science.gov (United States)

    Agapiou, A; Zorba, E; Mikedi, K; McGregor, L; Spiliopoulou, C; Statheropoulos, M

    2015-07-01

    Field experiments were devised to mimic the entrapment conditions under the rubble of collapsed buildings aiming to investigate the evolution of volatile organic compounds (VOCs) during the early dead body decomposition stage. Three pig carcasses were placed inside concrete tunnels of a search and rescue (SAR) operational field terrain for simulating the entrapment environment after a building collapse. The experimental campaign employed both laboratory and on-site analytical methods running in parallel. The current work focuses only on the results of the laboratory method using thermal desorption coupled to comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry (TD-GC×GC-TOF MS). The flow-modulated TD-GC×GC-TOF MS provided enhanced separation of the VOC profile and served as a reference method for the evaluation of the on-site analytical methods in the current experimental campaign. Bespoke software was used to deconvolve the VOC profile to extract as much information as possible into peak lists. In total, 288 unique VOCs were identified (i.e., not found in blank samples). The majority were aliphatics (172), aromatics (25) and nitrogen compounds (19), followed by ketones (17), esters (13), alcohols (12), aldehydes (11), sulfur (9), miscellaneous (8) and acid compounds (2). The TD-GC×GC-TOF MS proved to be a sensitive and powerful system for resolving the chemical puzzle of above-ground "scent of death".

  4. Fast Detection of Phenolic Compounds in Extracts of Easter Pears (Pyrus communis) from the Atacama Desert by Ultrahigh-Performance Liquid Chromatography and Mass Spectrometry (UHPLC-Q/Orbitrap/MS/MS).

    Science.gov (United States)

    Simirgiotis, Mario J; Quispe, Cristina; Bórquez, Jorge; Areche, Carlos; Sepúlveda, Beatriz

    2016-01-01

    A small Chilean variety of pears growing in the town of Toconao, an oasis located at the northeastern edge of the Salar de Atacama, northern Chile, was studied by means of modern PDA and high resolution mass spectral data (UHPLC-PDA-HESI-orbitrap-MS/MS). In addition, the antioxidant features of the fruits were compared with the varieties Packhman's Triumph and Abate Fetel and correlated with the presence of phenolic compounds. The non-pigmented phenolics were fingerprinted and related to the antioxidant capacities measured by the bleaching of the DPPH radical, the ferric reducing antioxidant power (FRAP), the superoxide anion scavenging activity assay (SA), and total content of phenolics and flavonoids measured by spectroscopic methods. The machine allowed a fast separation of 15 min employing a flow rate of 1 mL per minute and could accurately identify 25 compounds, including several isorhamnetin derivatives and phenolic acids, present in the peel and pulps of this Chilean variety for the first time. The compounds were monitored using a wavelength range of 210-800 nm. The native small Chilean pear showed the highest antioxidant activity measured as the bleaching of the DPPH radical, the ferric reducing antioxidant power and superoxide anion scavenging activity (8.61 ± 0.65 μg/mL, 712.63 ± 12.12 micromols trolox equivalents (μmol/TE)/100 g FW, and 82.89% ± 2.52% at 100 μg/mL, respectively). PMID:26784158

  5. 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 capture greater than 90 percent of sulfur gases evolved during thermal treatment of lunar soils....

  6. Dosimetric implications of new compounds for neutron capture therapy (NCT)

    Energy Technology Data Exchange (ETDEWEB)

    Fairchild, R.G.

    1982-01-01

    Systemic application of radiolabeled or cytotoxic agents should allow targeting of primary and metastatic neoplasms on a cellular level. In fact, drug uptake in non-target cell pools often exceeds toxic levels before sufficient amounts are delivered to tumor. In addition, at the large concentration of molecules necessary for therapy, effects of saturation are often found. Application of NCT can circumvent problems associated with high uptake in competing non-target cell pools, as the /sup 10/B(n,..cap alpha..)/sup 7/Li reaction is activated only within the radiation field. A comparison with other modes of particle therapy indicated that NCT provides significant advantages. It is however, difficult to obtain vehicles for boron transport which demonstrate both the tumor specificity and concentration requisite for NCT. A number of biomolecules have been investigated which show both the necessary concentration and specificity. These include chlorpromazine, thiouracil, porphyrins, amino acids, and nucleosides. However, these analogs have yet to be made available for NCT. Dosimetric implications of binding sites are considered, as well as alternate neutron sources. (ERB)

  7. Estimation of transport parameters of phenolic compounds and inorganic contaminants through composite landfill liners using one-dimensional mass transport model

    International Nuclear Information System (INIS)

    Highlights: → We conduct 1D advection-dispersion modeling to estimate transport parameters. → We examine fourteen phenolic compounds and three inorganic contaminants. → 2-MP, 2,4-DCP, 2,6-DCP, 2,4,5-TCP, 2,3,4,6-TeCP have the highest coefficients. → Dispersion coefficients of Cu are determined to be higher than Zn and Fe. → Transport of phenolics can be prevented by zeolite and bentonite in landfill liners. - Abstract: One-dimensional (1D) advection-dispersion transport modeling was conducted as a conceptual approach for the estimation of the transport parameters of fourteen different phenolic compounds (phenol, 2-CP, 2-MP, 3-MP, 4-MP, 2-NP, 4-NP, 2,4-DNP, 2,4-DCP, 2,6-DCP, 2,4,5-TCP, 2,4,6-TCP, 2,3,4,6-TeCP, PCP) and three different inorganic contaminants (Cu, Zn, Fe) migrating downward through the several liner systems. Four identical pilot-scale landfill reactors (0.25 m3) with different composite liners (R1: 0.10 + 0.10 m of compacted clay liner (CCL), Le = 0.20 m, ke = 1 x 10-8 m/s, R2: 0.002-m-thick damaged high-density polyethylene (HDPE) geomembrane overlying 0.10 + 0.10 m of CCL, Le = 0.20 m, ke = 1 x 10-8 m/s, R3: 0.002-m-thick damaged HDPE geomembrane overlying a 0.02-m-thick bentonite layer encapsulated between 0.10 + 0.10 m CCL, Le = 0.22 m, ke = 1 x 10-8 m/s, R4: 0.002-m-thick damaged HDPE geomembrane overlying a 0.02-m-thick zeolite layer encapsulated between 0.10 + 0.10 m CCL, Le = 0.22 m, ke = 4.24 x 10-7 m/s) were simultaneously run for a period of about 540 days to investigate the nature of diffusive and advective transport of the selected organic and inorganic contaminants. The results of 1D transport model showed that the highest molecular diffusion coefficients, ranging from 4.77 x 10-10 to 10.67 x 10-10 m2/s, were estimated for phenol (R4), 2-MP (R1), 2,4-DNP (R2), 2,4-DCP (R1), 2,6-DCP (R2), 2,4,5-TCP (R2) and 2,3,4,6-TeCP (R1). For all reactors, dispersion coefficients of Cu, ranging from 3.47 x 10-6 m2/s to 5.37 x 10-2 m2/s, was

  8. Capture and fission with DANCE and NEUANCE

    Energy Technology Data Exchange (ETDEWEB)

    Jandel, M.; Baramsai, B.; Bond, E.; Rusev, G.; Walker, C.; Bredeweg, T.A.; Chadwick, M.B.; Couture, A.; Fowler, M.M.; Hayes, A.; Kawano, T.; Mosby, S.; Stetcu, I.; Taddeucci, T.N.; Talou, P.; Ullmann, J.L.; Vieira, D.J.; Wilhelmy, J.B. [Los Alamos National Laboratory, Los Alamos, New Mexico (United States)

    2015-12-15

    A summary of the current and future experimental program at DANCE is presented. Measurements of neutron capture cross sections are planned for many actinide isotopes with the goal to reduce the present uncertainties in nuclear data libraries. Detailed studies of capture gamma rays in the neutron resonance region will be performed in order to derive correlated data on the de-excitation of the compound nucleus. New approaches on how to remove the DANCE detector response from experimental data and retain the correlations between the cascade gamma rays are presented. Studies on {sup 235}U are focused on quantifying the population of short-lived isomeric states in {sup 236}U after neutron capture. For this purpose, a new neutron detector array NEUANCE is under construction. It will be installed in the central cavity of the DANCE array and enable the highly efficient tagging of fission and capture events. In addition, developments of fission fragment detectors are also underway to expand DANCE capabilities to measurements of fully correlated data on fission observables. (orig.)

  9. Capture and fission with DANCE and NEUANCE

    Science.gov (United States)

    Jandel, M.; Baramsai, B.; Bond, E.; Rusev, G.; Walker, C.; Bredeweg, T. A.; Chadwick, M. B.; Couture, A.; Fowler, M. M.; Hayes, A.; Kawano, T.; Mosby, S.; Stetcu, I.; Taddeucci, T. N.; Talou, P.; Ullmann, J. L.; Vieira, D. J.; Wilhelmy, J. B.

    2015-12-01

    A summary of the current and future experimental program at DANCE is presented. Measurements of neutron capture cross sections are planned for many actinide isotopes with the goal to reduce the present uncertainties in nuclear data libraries. Detailed studies of capture gamma rays in the neutron resonance region will be performed in order to derive correlated data on the de-excitation of the compound nucleus. New approaches on how to remove the DANCE detector response from experimental data and retain the correlations between the cascade gamma rays are presented. Studies on 235U are focused on quantifying the population of short-lived isomeric states in 236U after neutron capture. For this purpose, a new neutron detector array NEUANCE is under construction. It will be installed in the central cavity of the DANCE array and enable the highly efficient tagging of fission and capture events. In addition, developments of fission fragment detectors are also underway to expand DANCE capabilities to measurements of fully correlated data on fission observables.

  10. Capture and fission with DANCE and NEUANCE

    International Nuclear Information System (INIS)

    A summary of the current and future experimental program at DANCE is presented. Measurements of neutron capture cross sections are planned for many actinide isotopes with the goal to reduce the present uncertainties in nuclear data libraries. Detailed studies of capture gamma rays in the neutron resonance region will be performed in order to derive correlated data on the de-excitation of the compound nucleus. New approaches on how to remove the DANCE detector response from experimental data and retain the correlations between the cascade gamma rays are presented. Studies on 235U are focused on quantifying the population of short-lived isomeric states in 236U after neutron capture. For this purpose, a new neutron detector array NEUANCE is under construction. It will be installed in the central cavity of the DANCE array and enable the highly efficient tagging of fission and capture events. In addition, developments of fission fragment detectors are also underway to expand DANCE capabilities to measurements of fully correlated data on fission observables. (orig.)

  11. Determination of quaternary ammonium compounds in oranges and cucumbers using QuEChERS extraction and ultra-performance liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Arrebola-Liébanas, Francisco Javier; Abdo, María Angeles Herrera; Moreno, José Luis Fernandez; Martínez-Vidal, José L; Frenich, Antonia Garrido

    2014-01-01

    A simple and fast method has been developed for determining relevant quaternary ammonium compounds in cucumber and orange samples. The target compounds were benzoalkonium chloride (BAC-10, BAC-12, BAC-14, and BAC-16), didecyldimethylammonium chloride, and benzethonium chloride, all frequently used biocides in the agrifood industry. An extraction based on the buffered Quick, Easy, Cheap, Effective, Rugged, and Safe method and determination by ultra-performance LC/MS/MS that eluted the biocides in less than 5 min were used. The method was fully validated and implemented in a UNE-EN-ISO/IEC 17025 accredited laboratory for its application to the analysis of real samples. Performance characteristics of the method are reported, including an estimation of measurement uncertainty. Calibration curves were set between 0.01 and 0.150 mg/kg, LOD values were always between 0.4 and 1.0 microg/kg, LOQ values were in the range 1-4 microg/kg, recovery was between 81 and 115%, intraday and interday precision were always lower than 17% (expressed as RSD), and expanded uncertainty was always lower than 40%. The validation was accomplished for the two studied matrixes at spiking concentrations of 0.011 and 0.050 mg/kg. The method has been applied to the analysis of 30 cucumber and orange samples that were found to contain concentrations of BAC-12 that ranged between 0.015 and 0.210 mg/kg and of BAC-14 between 0.018 and 0.081 mg/kg. PMID:25145132

  12. 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

    DEFF Research Database (Denmark)

    Pedersen, Gitte Alsing; Larsen, Erik Huusfeldt

    1997-01-01

    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-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...

  13. Synovectomy by Neutron capture

    International Nuclear Information System (INIS)

    The Synovectomy by Neutron capture has as purpose the treatment of the rheumatoid arthritis, illness which at present does not have a definitive curing. This therapy requires a neutron source for irradiating the articulation affected. The energy spectra and the intensity of these neutrons are fundamental since these neutrons induce nuclear reactions of capture with Boron-10 inside the articulation and the freely energy of these reactions is transferred at the productive tissue of synovial liquid, annihilating it. In this work it is presented the neutron spectra results obtained with moderator packings of spherical geometry which contains in its center a Pu239 Be source. The calculations were realized through Monte Carlo method. The moderators assayed were light water, heavy water base and the both combination of them. The spectra obtained, the average energy, the neutron total number by neutron emitted by source, the thermal neutron percentage and the dose equivalent allow us to suggest that the moderator packing more adequate is what has a light water thickness 0.5 cm (radius 2 cm) and 24.5 cm heavy water (radius 26.5 cm). (Author)

  14. Capturing lightness between contours.

    Science.gov (United States)

    Vergeer, Mark; van Lier, Rob

    2010-01-01

    Homogeneously coloured bars may exhibit lightness differences at the intersections. A well-known e