Derivatization and Analysis of Oligosaccharides by Matrix-assisted Laser Desorption/Ionization Time of-Flight Mass Spectrometry

Abstract Based on a labeling regent1-(4-Cyanophenyl)-4-piperidinecarbohydrazide(CPH), a derivatization method was developed for the determination of oligosaccharides with high sensitivity by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS). The hydrazones were generated by the reaction of the reducing ends of oligosaccharides and the hydrazide of CPH. The derivatives were directly analyzed by MALDI-TOF-MS. Reaction conditions such as reaction temperature, concentration of acetic acid, and excess ratio of CPH regent were optimized. When the oligosaccharides reacted with 100-fold excess of CPH at 100 °C and in 0.125% ( V / V ) acetic acid, the yield was the highest. The results showed that the derivatization with CPH increased the sensitivity of MS detection, and this method was suitable for the analysis of oligosaccharides' compositions.