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Herein, a structurally well\u2010defined porous heterojunction matrix, COF316@CuHHTP, is developed through an in situ epitaxial\u2010growth strategy for serum metabolomic screening. Porous and chemically robust COF316 serves as the core scaffold, while conductive CuHHTP forms a coherent shell for interfacial charge mediation. The resulting heterojunction enables efficient small\u2010molecule capture and directional transport through the channels, while enhanced photothermal conversion and optimized charge transport collectively improve desorption\/ionization efficiency and sensitivity for small\u2010molecule metabolites. Consequently, COF316@CuHHTP enables sensitive and robust laser desorption\/ionization mass spectrometry (LDI\u2010MS) analysis, with the maximum signal\u2010to\u2010noise (S\/N) enhancement reaching \u223c194\u2010fold, ultralow limits of detection (LODs) down to the pmol level, and strong tolerance to high\u2010salt and protein\u2010rich conditions. Applied to serum analysis, this platform enables BC diagnosis with excellent discriminatory performance (AUC = 0.996) and identifies 20 disease\u2010associated metabolic signatures.<\/jats:p>","DOI":"10.1002\/adma.74620","type":"journal-article","created":{"date-parts":[[2026,8,12]],"date-time":"2026-08-12T09:39:21Z","timestamp":1786527561000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Porous COF@cMOF Heterojunction\u2010Assisted Laser Desorption\/Ionization Mass Spectrometry for Enhanced Breast\u2010Cancer Serum Metabolomic Screening"],"prefix":"10.1002","volume":"38","author":[{"ORCID":"https:\/\/orcid.org\/0009-0002-5158-6331","authenticated-orcid":false,"given":"Yingxue","family":"Jin","sequence":"first","affiliation":[{"name":"State Key Laboratory of Chemistry for NBC Hazards Protection College of Chemistry Fuzhou University  Fuzhou China"},{"name":"Ministry of Education Key Laboratory of Analytical 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