Recently, Professor Ying Wang has published research findings in Nature Communications. This study proposed a microfluidic-based strategy for compositional regulation of electrochemical diffusion layer, and developed a multi-component forced convection electrochemical mass spectrometry. This technique precisely controlled the isotopic abundance of adsorbed oxygen (*O) and free water within the diffusion layer, thereby forming *O-labeled interfaces with specific coverages. It revealed the mechanism by which the oxygen evolution reaction pathway contributed to the overpotential through tracking *O conversions. This work offered a new approach for elucidating the conversion pathways of electrochemical intermediates.