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[Display omitted] • Operando NMR combined with gas-probe method was used to study active sites transfer under the metal-support interaction. • The photocatalytic conversion efficiency of pure TiO 2 decreased, while that of Pt/TiO 2 was unaffected in gas conditions. • After loading metal-Pt, active sites changed from TiO 2 surface to Pt/TiO 2 interface. Recently metal-support interaction (MSI) has attracted considerable attention in photocatalysis. Some studies emphasize the importance of active sites on photocatalysts; however, there are no reports on site changes under MSI in real reactive conditions. Herein, an operando nuclear magnetic resonance technique was proposed to study such site changes on anatase TiO 2 and Pt/TiO 2 , through a gas-probe method, in CH 3 OH reforming. The photocatalytic oxidation efficiency of CH 3 OH by pure TiO 2 decreased immensely under extra-gas conditions, while that by Pt/TiO 2 was unaffected. The surface of pure TiO 2 were occupied by injected gas molecules, making CH 3 OH inaccessible to active sites. However, in Pt/TiO 2 , CH 3 OH adsorption sites changed from TiO 2 surface to metal-Pt/TiO 2 interface as confirmed by H 2 gas-probe experiments. This study provides a deeper understanding of active sites transfer by MSI and leverages the gas-probe method for its detection to guide the development of technology to test active-site positions in heterogeneous catalysts. [ABSTRACT FROM AUTHOR]