Journal of the Mass Spectrometry Society of Japan
Online ISSN : 1880-4225
Print ISSN : 1340-8097
ISSN-L : 1340-8097
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Volume 38, Issue 2
Displaying 1-4 of 4 articles from this issue
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REGULAR PAPERS
  • Large Sample Volume Injection on Capillary GC/MS
    Part 1: Jet Separator as GC/MS Interface
    Chuichi Watanabe, Keiji Hashimoto
    1990 Volume 38 Issue 2 Pages 65-70
    Published: 1990
    Released on J-STAGE: May 01, 2007
    DOIhttps://doi.org/10.5702/massspec.38.65
    JOURNAL FREE ACCESS
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    Large sample volume injection method, 10 to 100 μl, into a capillary column using a packed column injector has many advantages over such ordinary injection methods as split and splitless injections. In order to apply this injection system to a magnetic sector-type mass spectrometer, a jet separator with a solvent cut shutter slit between a jet nozzle and an ion source is selected as a GC/MS interface. As a result, the detection limit was remarkably improved over 10 times in both TIC and SIM detection modes. For example, the detection limits for the methyl stearate by injecting 50 μl of the sample were 50 ppb and 10 ppt in TIC and SIM modes, respectively. The problems to be improved are also discussed.
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  • Type Analysis of Hydrocarbons in Condensate Oils by Chemical Ionization Mass Spectrometry
    Shizuko Okada, Shigeki Daishima, Yoshio Iida, Machiko Tezuka
    1990 Volume 38 Issue 2 Pages 71-76
    Published: 1990
    Released on J-STAGE: May 01, 2007
    DOIhttps://doi.org/10.5702/massspec.38.71
    JOURNAL FREE ACCESS
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    A simple and rapid method for the determination of paraffins (PA), cycloparaffins (CY), and aromatic hydrocarbons (AR) was developed by chemical ionization mass spectrometry, and applied to type analysis of condensate oils which contained little oleffins. After 0.200 ml of p-xylene-d10 was added to 1.80 ml of condensate oil as an internal standard, 0.05 μl of the sample was introduced into a GC/MS equipped with a capillary column (0.25 mm i. d. × 15 m) at the split ratio of 10 : 1. The reconstructed mass spectra were obtained by monitoring the characteristic ions, such as (M±H)+, CnH2n+1+ etc., with a methane reagent gas. The concentrations of PA, CY, and AR were calculated from simultaneous equations equal to numbers of components to be determined, which set up by assuming additivity of the peak intensities. Analytical results were in satisfactory agreement with those obtained by the modified method of the fluorescent indicator adsorption (FIA) method for condensate oils. The measurement time by the present method was ca. 5 min in contrast with ca. 6 h of the modified FIA method.
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  • A New Matrix System in Fast Atom Bombardment Mass Spectrometry of Prenylated- and Geranylated-Phenolic Compounds
    Mitsuo Takayama, Toshio Fukai, Yoshio Hano, Taro Nomura
    1990 Volume 38 Issue 2 Pages 77-85
    Published: 1990
    Released on J-STAGE: May 01, 2007
    DOIhttps://doi.org/10.5702/massspec.38.77
    JOURNAL FREE ACCESS
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    A 1 : 1 (v/v) mixture of m-nitrobenzyl alcohol (m-NBA) and 2,2'-dithiodiethanol (DTDE, HOCH2CH2SSCH2CH2OH) was applied as a new matrix system to FAB mass spectra of prenylated- and geranylated-phenolic compounds, with which the matrix was relatively involatile and durable for a long period of time. This resulted in the good reproducibility of the FAB spectra. The FAB spectra were compared with the corresponding EI and CI mass spectra. The FAB spectra gave the intense molecular ions M+· and the fragment ions.
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  • Determination of Hippuric Acid in Urine by GC/MS:
    in vivo Metabolism of Toluene to Hippuric Acid on Toluene Poisoning
    Hidemi Todoriki, Tokishi Hayashi, Hiromi Gunshin, Dalmas A. R. Dominic ...
    1990 Volume 38 Issue 2 Pages 87-94
    Published: 1990
    Released on J-STAGE: May 01, 2007
    DOIhttps://doi.org/10.5702/massspec.38.87
    JOURNAL FREE ACCESS
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    This paper describes the use of the stable isotope tracer method for the metabolism from toluene to hippuric acid to help an assessing biological monitoring at low level exposure of toluene. This analytical method was applied to Wistar rats with poisoning of toluene during two weeks period, and was used to determine the urinary levels of endogeneous hippuric acid-d0 and exogenous hippuric acid-d5 which is produced from toluene-d8 in vivo, after intra-peritoneal administration of toluene-d8. It was possible to detect an alteration in the excretion of urinary hippuric acid compared with the control using deuterium-labeled toluene as a stable isotope tracer to distinguish its metabolite from endogeneous metabolite. We suggest that the in vivo metabolic investigation of the biological monitoring for hippuric acid should be based on the stable isotope method, and that the method was effective for the measurement of low exposure concentrations.
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