Publication date: 15th May 2025
Metal–organic frameworks (MOFs) are an emerging class of nanozymes, with metal oxyhydroxide (MOOH)-based nodes acting as primary catalytic sites. In this study, we report that hybrid ZrOOH@COF15 structures, constructed by anchoring open and uncoordinated ZrOOH species onto a covalent organic framework (COF), exhibit significantly enhanced catalytic activity for cysteine disulfide bond formation (DBF) compared to reported catalysts such as Ce-POMs, CeO2, and Ce/Zr-UiO-66 MOFs. ¹H NMR spectroscopy revealed that ZrOOH@COF15 displayed sixfold higher reactivity compared to pristine COF15, achieving 100% selective conversion to cystine. Notably, ZrOOH alone exhibited no detectable catalytic activity. Contrary to previous reports, no DBF was observed in the absence of a catalyst under acidic, neutral, or basic pH conditions over a reaction period of 3 hours, confirming that cystine formation was exclusively catalyzed by ZrOOH@COF15. While an increase in pH enhanced catalytic cysteine DBF activity, suppression of the reaction was observed when each parameter was individually modified: nitrogen purging, exclusion of ambient light, or addition of the superoxide scavenger hydroquinone. Mechanistically, catalysis begins with the adsorption of cysteine onto the Zr-metal center, followed by thiol ionization, facilitated by synergistic interactions between the metal center and alkaline pH. Our studies indicate that the COF15 plays a pivotal role in catalysis via the activation of dissolved molecular oxygen, which then oxidizes cysteinyl anions to form cysteinyl radicals. These radicals subsequently undergo homonuclear coupling to yield cystine. Kinetic studies revealed a saturation-limited catalytic profile for ZrOOH@COF15, while thermodynamic analysis indicated that its enhanced activity stems from a reduced overall activation barrier, driven by synergistic interplay between the Zr center and the COF framework. Overall, ZrOOH@COF15 functions as a highly efficient dual-active-site catalyst for the selective formation of cysteine DBF.
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