A novel mass spectrometric procedure for the rapid determination of the types of carbohydrate chains present in glycoproteins: Application to α-galactosidase I from Vicia faba seeds

Combined Partial Acid Hydrolysis and Electrospray Ionization-Mass Spectrometry for the Structural Determination of Oligosaccharides

“…Mass spectrometry is becoming the method of choice for the analysis of oligosaccharides. ,− Unfortunately, use of traditional methods of acid hydrolysis (mineral acids and trifluoroacetic acid (TFA)) is not compatible with electrospray ionization mass spectrometry (ESI-MS) without tedious cleanup procedures. Fast-atom bombardment mass spectrometry has been previously applied to the acetolysis products of acetylated oligosaccharides, , but investigation of the acid hydrolysis products of native oligosaccharides with ESI-MS has not been reported. In the study described herein, a method is introduced that utilizes an acid-exchange resin as the catalyst for the hydrolysis of oligosaccharides; the products of which are directly amenable to ESI-MS. We also demonstrate that the hydrolysate products are efficiently removed from the acid source by simple filtration and that partial acid hydrolysis of an oligosaccharide generates a reducing end ladder sequence in solution that is easily detected by mass spectrometry.…”