期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1194, 期 2, 页码 237-242出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2008.04.050
关键词
capillary electrophoresis-mass spectrometry; sulfated glycopeptides; selective enrichment; ion-pair reaction
We describe a new capillary electrophoresis-mass spectrometry (CE-MS)-based technique for analyzing sulfated glycopeptides. The proposed method performs selective enrichment of sulfated glycopeptides from a complex mixture of peptides based on field-enhanced sample injection and ion-pair reaction with a basic ion-pair reagent (Lys-Lys-Lys; KKK) at the exit end of a capillary in a single analysis, which permits successful fragmentation of sulfated glycopeptides in positive-ion mode at the MS/MS stage for comprehensive structural analysis. In this study, the method was verified using a model sulfated monosaccharide, N-acetyl-D-galactosamine 4-sulfate (GalNAc 4S). As an example of an application of this method, sulfated glycopeptides were selectively enriched from the enzymatic digest of thyroid stimulating hormone, affording similar to 500-fold sensitivity enhancement, and structural information was successfully obtained via on-line ion-pair complexation reaction. (c) 2008 Elsevier B.V. All rights reserved.
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