Complete mass spectral characterization of a synthetic ultralow-molecular-weight heparin using collision-induced dissociation.
Anal Chem
; 84(13): 5475-8, 2012 Jul 03.
Article
em En
| MEDLINE
| ID: mdl-22715938
ABSTRACT
Glycosaminoglycans (GAGs) are a class of biologically important molecules, and their structural analysis is the target of considerable research effort. Advances in tandem mass spectrometry (MS/MS) have recently enabled the structural characterization of several classes of GAGs; however, the highly sulfated GAGs, such as heparins, have remained a relatively intractable class due their tendency to lose SO(3) during MS/MS, producing few sequence-informative fragment ions. The present work demonstrates for the first time the complete structural characterization of the highly sulfated heparin-based drug Arixtra. This was achieved by Na(+)/H(+) exchange to create a more ionized species that was stable against SO(3) loss, and that produced complete sets of both glycosidic and cross-ring fragment ions. MS/MS enables the complete structural determination of Arixtra, including the stereochemistry of its uronic acid residues, and suggests an approach for solving the structure of more complex, highly sulfated heparin-based drugs.
Texto completo:
1
Coleções:
01-internacional
Base de dados:
MEDLINE
Assunto principal:
Polissacarídeos
/
Heparina de Baixo Peso Molecular
/
Espectrometria de Massas em Tandem
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Anticoagulantes
Idioma:
En
Ano de publicação:
2012
Tipo de documento:
Article