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Structural analysis of permethylated oligosaccharides using electrospray ionization quadrupole time‐of‐flight tandem mass spectrometry and deutero‐reduction

Structural analysis of permethylated oligosaccharides using electrospray ionization quadrupole... Deutero‐reduced permethylated oligosaccharides were analyzed by electrospray ionization mass spectrometry (ESI‐MS) and tandem mass spectrometry (MS/MS) using a hybrid quadrupole orthogonal acceleration time‐of‐flight mass spectrometer, fitted with a nanoflow ESI source. Under these ionization conditions such derivatives preferentially form sodiated molecular species in addition to protonated molecular species. Under collision‐induced dissociation, protonated and sodiated molecular species yield simple and predictable fragment mass spectra. A systematic study was conducted on a series of deutero‐reduced permethylated glycans to allow rationalization of the fragmentation processes. MS/MS spectra were characterized by fragments resulting from the cleavage of glycosidic bonds. These fragments originating from both the reducing and the non‐reducing ends of the glycan yield information on sequence and branching. Furthermore, the substituent 3‐linked to a HexNAc unit was readily eliminated. Special attention was devoted to a systematic study of fucosylated glycans. The fucosylated deutero‐reduced permethylated glycans were submitted to an acidic hydrolysis, releasing specifically the fucosyl residues. The nascent free hydroxyl groups were subsequently CD3‐labelled in order to determine the positions initially bearing the fucosyl residues along the oligosaccharide backbone. This methodology was finally applied to characterize a glycan pool enzymatically released from glycoproteins. The present data show that structural elucidation can be achieved at the 50 fmol level. Copyright © 2004 John Wiley & Sons, Ltd. http://www.deepdyve.com/assets/images/DeepDyve-Logo-lg.png Rapid Communications in Mass Spectrometry Wiley

Structural analysis of permethylated oligosaccharides using electrospray ionization quadrupole time‐of‐flight tandem mass spectrometry and deutero‐reduction

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References (44)

Publisher
Wiley
Copyright
Copyright © 2004 Wiley Subscription Services
ISSN
0951-4198
eISSN
1097-0231
DOI
10.1002/rcm.1640
pmid
15384134
Publisher site
See Article on Publisher Site

Abstract

Deutero‐reduced permethylated oligosaccharides were analyzed by electrospray ionization mass spectrometry (ESI‐MS) and tandem mass spectrometry (MS/MS) using a hybrid quadrupole orthogonal acceleration time‐of‐flight mass spectrometer, fitted with a nanoflow ESI source. Under these ionization conditions such derivatives preferentially form sodiated molecular species in addition to protonated molecular species. Under collision‐induced dissociation, protonated and sodiated molecular species yield simple and predictable fragment mass spectra. A systematic study was conducted on a series of deutero‐reduced permethylated glycans to allow rationalization of the fragmentation processes. MS/MS spectra were characterized by fragments resulting from the cleavage of glycosidic bonds. These fragments originating from both the reducing and the non‐reducing ends of the glycan yield information on sequence and branching. Furthermore, the substituent 3‐linked to a HexNAc unit was readily eliminated. Special attention was devoted to a systematic study of fucosylated glycans. The fucosylated deutero‐reduced permethylated glycans were submitted to an acidic hydrolysis, releasing specifically the fucosyl residues. The nascent free hydroxyl groups were subsequently CD3‐labelled in order to determine the positions initially bearing the fucosyl residues along the oligosaccharide backbone. This methodology was finally applied to characterize a glycan pool enzymatically released from glycoproteins. The present data show that structural elucidation can be achieved at the 50 fmol level. Copyright © 2004 John Wiley & Sons, Ltd.

Journal

Rapid Communications in Mass SpectrometryWiley

Published: Jan 30, 2004

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