The results of this experiment confirm that the generation of peeling reaction products, which are an artefact that is problematic when attempting to perform accurate O-glycan profiling, can be suppressed to a few percent of the total O-glycans by carrying out One-pod PMP labeling using ammonium carbamate. Although there are restrictions such as the amount of samples required, this method can be used for O-glycan profiling. However, the reagent and reaction conditions that were used in this study gave a glycan release efficiency and labeling efficiency that were not high when compared with other methods. The technique of simultaneously accomplishing glycan release and labeling is effective in terms of suppressing the peeling reaction. For PMP labeling, however, detection with LC is based on UV absorbance, and the detection sensitivity is low in comparison with fluorescence detection such as for PA labeling and 2-AB labeling, and there is susceptibility to background effects due to contaminant reagents. In order to eliminate these effects, it is necessary to investigate reagents with good reaction efficiency that can simultaneously perform releasing and labeling, and to conduct further studies on the reaction conditions.