Chip‐based CE coupled to a quadrupole TOF mass spectrometer for the analysis of a glycopeptide

A novel approach using sheath flow chip‐based CE coupled to a quadrupole TOF mass spectrometer was developed and applied to the analysis of an O‐glycopeptide. The method provided good separation and sensitive analysis of the glycopeptide and its β‐elimination product. The β‐elimination reaction of the glycopeptide with ammonia or dimethylamine was adapted for changing the glycopeptide into deglycosylated form and for specifying the site of glycosylation. MS/MS analysis of the native peptide, glycopeptide and β‐elimination product enabled the identification of the glycosylation site through the comparison of the fragmentations and peptide sequence analysis.

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