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Here, a stable water-in-oil-in-water multicompartment Pickering emulsion was constructed through the synergistic coassembly of polyvinylpyrrolidone-modified gold nanoparticles (Au@PVP) and bovine serum albumin (BSA). The suitable wettability of Au@PVP, together with BSA adsorption and reorganization, promoted the formation of a dense composite nanoparticle film at the oil\u2013water interface, enabling long-term emulsion stability. Using the BSA-catalyzed condensation of chalcone and malononitrile as a model reaction, in situ surface-enhanced Raman spectroscopy (SERS) revealed significantly enhanced interfacial reaction kinetics compared with those in the monolayer emulsion system, with the target product yield increasing by approximately 6.8-fold after 24 h. Fourier transform infrared spectroscopy independently confirmed the kinetic trend. For bioanalysis, replacing BSA with cell-secreted components generated functional emulsion substrates with highly reproducible SERS signals. Combined with feed-forward neural network analysis, the platform achieved classification accuracies exceeding 95% for three types of extracellular vesicles. This multicompartment emulsion platform integrates interfacial engineering, reaction acceleration, real-time monitoring, and intelligent biosensing, providing a versatile strategy for organic catalysis, biomarker detection, and liquid biopsy.<\/jats:p>","DOI":"10.1021\/acs.analchem.6c03152","type":"journal-article","created":{"date-parts":[[2026,9,20]],"date-time":"2026-09-20T14:01:43Z","timestamp":1789912903000},"page":"28872-28881","source":"Crossref","is-referenced-by-count":1,"title":["Multiple Pickering\nEmulsions Enable Highly Efficient\nInterfacial Catalysis and Extracellular Vesicle Classification via\nIn Situ Surface-Enhanced Raman Spectroscopy"],"prefix":"10.1021","volume":"98","author":[{"given":"Yaguang","family":"Yin","sequence":"first","affiliation":[{"name":"Hefei University of Technology , , ,","place":["Hefei, P. R. China, 230601"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Cheng","family":"Wang","sequence":"additional","affiliation":[{"name":"Hefei University of Technology , , ,","place":["Hefei, P. R. China, 230601"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0910-2444","authenticated-orcid":true,"given":"Honglin","family":"Liu","sequence":"additional","affiliation":[{"name":"Hefei University of Technology , , ,","place":["Hefei, P. R. China, 230601"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,9,20]]},"reference":[{"issue":"30","key":"2026100608074078000_cit1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202115885","article-title":"Pickering Emulsion\nCatalysis: Interfacial Chemistry, Catalyst Design, Challenges, and\nPerspectives","volume":"61","author":"Ni","year":"2022","journal-title":"Angew. Chem., Int. 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Chem. Soc."},{"issue":"47","key":"2026100608074078000_cit31","doi-asserted-by":"publisher","first-page":"26141","DOI":"10.1021\/acs.analchem.5c05040","article-title":"AI-Enhanced Rapid\nSERS Screening of Trace Quinolone Antibiotics across the Source-Pathway-Sink\nEcosystem","volume":"97","author":"Xu","year":"2025","journal-title":"Anal. 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Sci."},{"key":"2026100608074078000_cit37","doi-asserted-by":"publisher","first-page":"153","DOI":"10.1016\/j.partic.2021.06.004","article-title":"Pickering emulsions\nstabilized by colloidal surfactants: Role of solid particles","volume":"64","author":"Sun","year":"2022","journal-title":"Particuology"},{"key":"2026100608074078000_cit38","doi-asserted-by":"publisher","first-page":"107","DOI":"10.1016\/j.jcis.2025.01.093","article-title":"Weakening\nCoulomb interactions in ionic liquid via hydrogen bonds enables ultrafast\nsupercapacitors","volume":"685","author":"Fan","year":"2025","journal-title":"J. Colloid Interface Sci."},{"key":"2026100608074078000_cit39","doi-asserted-by":"publisher","first-page":"12","DOI":"10.1016\/j.jechem.2021.10.029","article-title":"Improved crystallinity\nand self-healing effects in perovskite solar\ncells via functional incorporation of polyvinylpyrrolidone","volume":"68","author":"Niu","year":"2022","journal-title":"J. Energy Chem."},{"key":"2026100608074078000_cit40","doi-asserted-by":"publisher","first-page":"108294","DOI":"10.1016\/j.compscitech.2020.108294","article-title":"A self-healing, stretchable,\nand\nconductive Poly(N-vinylpyrrolidone)\/gallic acid composite hydrogel\nformed via hydrogen bonding for wearable electronic sensors","volume":"198","author":"Zhao","year":"2020","journal-title":"Compos. Sci. 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