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Herein, we developed a dual\u2010surfactant co\u2010templating strategy to construct Zr\u2010based HP metal\u2010alkyl\u2010thiol frameworks (HPMATFs), where the HP structure facilitated the encapsulation of bulky biomacromolecules while the integrated alkyl thiols greatly enhanced their affinity toward noble metals. The high density of hydrophilic moieties at the periphery of the composite micelles effectively anchored the Zr precursors, preventing phase separation and enabling precise control over the mesopore sizes from 3 to 40\u00a0nm. The abundant alkyl thiols in the framework enabled the successful introduction of uniformly dispersed gold nanoparticles (AuNPs) within the HPMATFs matrix. Such integration provided abundant plasmonic sites and open mesospaces for the free diffusion of target analytes, forming an effective surface\u2010enhanced Raman scattering (SERS) platform. Spatial co\u2010confinement of oxidases and the SERS probe ensured an immediate cascade reaction between proximal enzyme\u2010generated products and the SERS probe anchored on AuNPs, realizing specific and sensitive recognition of the substrate of the applied enzymes. By altering the loaded enzymes, such a sensory platform can be applied for the specific detection of diverse biomolecular targets, prefiguring their potential for point\u2010of\u2010care diagnostics.<\/jats:p>","DOI":"10.1002\/smtd.70744","type":"journal-article","created":{"date-parts":[[2026,6,3]],"date-time":"2026-06-03T08:41:30Z","timestamp":1780476090000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Dual\u2010Surfactant\u2010Directed Mesoporous Metal\u2010Alkyl\u2010Thiol Frameworks for Enzyme\u2010Au Nanoparticle\u2010Coupled SERS Biosensing"],"prefix":"10.1002","volume":"10","author":[{"given":"Ximeng","family":"Liu","sequence":"first","affiliation":[{"name":"School of Materials Science and Engineering Key Laboratory for Ultrafine Materials of Ministry of Education East China University of Science and Technology  Shanghai 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