Journal of the American Society for Mass Spectrometry

, Volume 10, Issue 12, pp 1285–1290

Structural validation of saccharomicins by high resolution and high mass accuracy fourier transform-ion cyclotron resonance-mass spectrometry and infrared multiphoton dissociation tandem mass spectrometry

  • Stone D. H. Shi
  • Christopher L. Hendrickson
  • Alan G. Marshall
  • Marshall M. Siegel
  • Fangming Kong
  • Guy T. Carter
Articles

DOI: 10.1016/S1044-0305(99)00108-7

Cite this article as:
Shi, S.D.H., Hendrickson, C.L., Marshall, A.G. et al. J Am Soc Mass Spectrom (1999) 10: 1285. doi:10.1016/S1044-0305(99)00108-7

Abstract

Exceptionally high mass resolving power and mass accuracy combined with tandem mass spectrometry (MSn) capability make Fourier transform ion cyclotron resonance mass spectrometry a powerful tool for structure verification and determination of biological macromolecules. By means of local internal calibration and electron mass correction, mass accuracy better than ±0.5 ppm was achieved for two oligosaccharide antibiotics, Saccharomicins A and B, consistent with the proposed elemental compositions based upon NMR data. High resolution and high mass accuracy MS/MS data were obtained for both oligosaccharides by use of infrared multiphoton dissociation (IRMPD) with a 40 W continuous-wave CO2 laser. The spectra were charge-state deconvolved by the “Z-score” algorithm to yield much simpler mass-only spectra. Sequences of 15 sugar residues could be confirmed from the charge state deconvolved accurate mass MS/MS spectra for Saccharomicins A and B, even without use of traditional prior permethylation. A fragment corresponding to an internal sugar loss rearrangement was observed by IRMPD and studied by collision activated dissociation MS4.

Copyright information

© American Society for Mass Spectrometry 1999

Authors and Affiliations

  • Stone D. H. Shi
    • 1
  • Christopher L. Hendrickson
    • 1
  • Alan G. Marshall
    • 1
  • Marshall M. Siegel
    • 2
  • Fangming Kong
    • 2
  • Guy T. Carter
    • 2
  1. 1.Center for Interdisciplinary Magnetic Resonance, National High Magnetic Field Laboratory, and Department of ChemistryFlorida State UniversityTallahasseeUSA
  2. 2.Lederle LaboratoriesWyeth-Ayerst ResearchPearl RiverUSA
  3. 3.Ion Cyclotron Resonance Program, National High Magnetic Field LaboratoryFlorida State UniversityTallahassee