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 |
| |
Authors: | Stone D H Shi Christopher L Hendrickson Alan G Marshall Marshall M Siegel Fangming Kong Guy T Carter |
| |
Institution: | 1. Center for Interdisciplinary Magnetic Resonance, National High Magnetic Field Laboratory, and Department of Chemistry, Florida State University, Tallahassee, Florida, USA 3. Lederle Laboratories, Wyeth-Ayerst Research, Pearl River, New York, USA
|
| |
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. |
| |
Keywords: | |
本文献已被 ScienceDirect SpringerLink 等数据库收录! |
|