Journal of the Mass Spectrometry Society of Japan
Online ISSN : 1880-4225
Print ISSN : 1340-8097
ISSN-L : 1340-8097
Volume 52, Issue 6
Displaying 1-5 of 5 articles from this issue
REGULAR PAPER
  • Yuuki NOGUCHI, Akio HAYASHI, Kazuo TSUJIMOTO, Keiko MIYABAYASHI, Taku ...
    2004 Volume 52 Issue 6 Pages 307-316
    Published: 2004
    Released on J-STAGE: October 28, 2005
    JOURNAL FREE ACCESS
    The structures of the polar lipids in halobacteria including their mutants were determined with ESI-MS and FAB-MS. The composition-analyses with ESI-MS gave the results fairly close to these with TLC analyses. The percentages of the composite polar lipids by the mass spectrometric analyses of Halobacterium salinarum S-9 were 20, 77, and 5% for glycolipid sulfate (S-TGD), methyl ester of phosphatidyl glycerophosphate (PGP-OMe), and phosphatidylglycerol (PG), respectively. The MS/MS analysis in the FAB-MS provided an analyzing tool for the structural elucidation of the functional groups in the lipids. Newly proposed methylation in the phosphate was investigated with stable isotope experiments. We found that the Australian halobacteria, Halorubrum sp. aus-1, mainly consist of an isolated glycolipid sulfate with two sugar parts of glucopyranoses. In relationship with the lipid-composition analysis, the chemotaxonomy of halobacteria was discussed. The methylation of the lipids was proved to be essentially independent of that in the photosensory protein of halobacteria on the basis of the wide distribution of the methylated lipids.
    Download PDF (365K)
  • Tomoyuki SHIBATA, Masako YOSHIKAWA
    2004 Volume 52 Issue 6 Pages 317-324
    Published: 2004
    Released on J-STAGE: October 28, 2005
    JOURNAL FREE ACCESS
    We developed a technique combining mass spectrometry with chemical separation to analyze Sm-Nd isotopic compositions of ultramafic rock samples, which have extremely high Mg and low Nd concentrations and are always difficult to analyze. In the case of ultramafic rocks, abundant Mg forms fluorides during decomposition by HF, and minor amounts of Sm and Nd are strongly partitioned into fluorides, which would be a significant reason of low recovery yields of these elements and obstructed to determine a reliable isotopic ratio of Nd and Sm. We introduced pre-decomposition by HCl prior to the conventional method by HF and HClO4 that made it possible to elevate recovery yield to 85%. On the other hand, replicate measurements of Nd standard solution (La Jolla) by changing the ion current of Nd+ and the amount of Nd indicate that reliable isotopic ratios are measured under the condition of >0.04×10-11 A of 144Nd+ ion current and >2 ng of Nd. By applying our method, we analyzed 143Nd/144Nd ratio and Sm and Nd concentrations of PCC-1, which is an ultramafic standard rock sample of United States Geological Survey. The results of our analysis were 0.512226±0.000026, 0.00551±0.00041, and 0.0278±0.0011 ppm, respectively. These results are the first report of 143Nd/144Nd ratio for PCC-1.
    Download PDF (314K)
  • Kozo MATSUMOTO, Aritaka MATSUNAMI, Hiroyuki OYAMA, Miho TANAKA, Kuniyu ...
    2004 Volume 52 Issue 6 Pages 325-327
    Published: 2004
    Released on J-STAGE: October 28, 2005
    JOURNAL FREE ACCESS
    We have applied MALDI/TOF MS to the analysis of metal oxides by using chelating agents as matrices. The identification of metals is performed without any complicated pretreatment. Moreover, the oxidation numbers of the metals are determinable by using suitable chelating reagents. This simple method is successfully applied to the analysis of metal elements in natural crystal stone (Pyrite, FeS2).
    Download PDF (122K)
  • Yuko FUKUYAMA, Yoshinao WADA, Yuzo YAMAZAKI, Noriyuki OJIMA, Masaki YA ...
    2004 Volume 52 Issue 6 Pages 328-338
    Published: 2004
    Released on J-STAGE: October 28, 2005
    JOURNAL FREE ACCESS
    Mass spectrometry (MS) is becoming an indispensable analytical tool for glycoproteomics, that is, for the analysis of glycan and protein structures of glycoproteins. While a simple and rapid MS method which can minimize troublesome procedures for sample preparation is desired, a single mass spectrometer to meet this demand has not been realized to date. We report here a procedure for the structure analysis of Ribonuclease B (RNase B) using the MS and MSn analyses of protonated ions ([M+H]+) and sodium-adducted ions ([M+Na]+) by a single MALDI-QIT-TOFMS. Five peaks were identified as a glycopeptide in mass spectra with 2,5-dihydroxybenzoic acid (DHBA) as a matrix for RNase B digests by Lysyl endopeptidase (Lys C) without desalting. All of the five [M+H]+ peaks were accompanied by [M+Na]+ peaks. The same fragment peaks were observed in low mass area of all MS/MS spectrum for each [M+H]+ or [M+Na]+ species. MSn analyses using [M+H]+ as a precursor ion provided the information of peptide sequence and glycosylation site, while fragments from [M+Na]+ showed oligosaccharide sequence. Finally, this technique using [M+H]+ and [M+Na]+ with MALDI-QIT-TOFMS realized an easy and high-throughput implementation of glycoprotein structure analyses.
    Download PDF (380K)
TECHNICAL REPORT
  • Yoshikuni NAKAJIMA, Hideki WADA, Hiroyuki MATUZAKI, Yoshimi SUZUKI
    2004 Volume 52 Issue 6 Pages 339-346
    Published: 2004
    Released on J-STAGE: October 28, 2005
    JOURNAL FREE ACCESS
    We examined an analytical procedure for accurate determination of 14C concentrations in elemental carbon (EC) of an aerosol in the atmosphere. When carbon dioxide released by a combustion of EC is converted to graphite for 14C measurement with accelerator mass spectrometry (AMS), sulfur, nitrogen and halogens coreleased impede the conversion to graphite. We examined an appropriate condition for effective formation of graphite on metallic Fe powder. We used Ag wire and Sulfix® for removing halogens and sulfur oxides and also used a reduced copper metal for reduction of nitrogen oxides to nitrogen gas. The following condition was used: 0.1 mm in diameter Ag wire of 100 cm and reduced copper metal of about 30 mg were added in a vycol tube with about 64 mg of CuO during the EC combustion at 900° for 1 hour. In addition, CO2 evolved was heated at 350° with Sulfix® of about 20 mg in a pyrex tube. We obtained a yield up to 70% during the process to convert EC to graphite. Δ14C values of EC in aerosol were measured for 3 sets of samples: two from mountainous areas of Ikawa and one from Mt. Norikura and an urban area, Shizuoka University. The Δ14C values of EC at Mt. Norikura, (ave. -636‰) were similar to those at Shizuoka University (ave. -717‰), while the Δ14C values in Ikawa (ave. -282‰ to ave. -349‰) were higher than those of the other sites.
    Download PDF (243K)
feedback
Top