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Glutamine (Gln) is known as an unstable compound and converts to pyroglutamate (pGlu) in water solvent. Gln degradation speed is depended on temperature, pH, and ion strength. However, quantitative analysis of Gln degradation using mass spectrometry was little information. In this study, we investigated the quantitative analysis of Gln degradation using capillary electrophoresis-mass spectrometry (CE-MS). 200 μM Gln solution was prepared and acquired using CE-MS for 7 days under 25 °C. The detected compounds were Gln, pGlu, and glutamate (Glu), and the product speed was -0.36 μM h-1, 0.41 μM h-1, and 0.02 μM h-1, respectively. It was shown that Gln was generally converted to pGlu at equally ratio.