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Herein, we report a microemulsion\u2010mediated in situ growth strategy to construct a magnetic core\u2013shell structure with a well\u2010ordered hierarchically porous MOF shell (denoted as FeM@PMOFs). Mercaptoacetic acid (MAA) serves as a molecular bridge to anchor Ce\n                    <jats:sup>3<\/jats:sup>\n                    <jats:sup>+<\/jats:sup>\n                    \/Ce\n                    <jats:sup>4<\/jats:sup>\n                    <jats:sup>+<\/jats:sup>\n                    onto Fe\n                    <jats:sub>3<\/jats:sub>\n                    O\n                    <jats:sub>4<\/jats:sub>\n                    surfaces, while a P123\/mesitylene soft\u2010template system guides the formation of hierarchical porosity. FeM@PMOFs exhibit uniform morphology, a shell thickness of about 46\u00a0nm, and hierarchical pore sizes (9\u201368\u00a0nm meso\/macropores together with 1.58\u00a0nm micropores). Leveraging hierarchically porous, excellent hydrophilicity owing to the MOF shells, and rapid magnetic separation, FeM@PMOFs enable selective and sensitive enrichment of N\u2010glycopeptides with an exceptionally low detection limit of 1 amol \u00b5L\n                    <jats:sup>\u22121<\/jats:sup>\n                    . When applied to human serum samples from healthy controls and patients with prostate, bladder, and renal cancers, the platform identified 324 unique N\u2010glycopeptides and revealed 20 candidate glycopeptide signatures distinguishing different urological malignancies. This work provides a generalizable synthetic strategy for ordered magnetic hierarchical MOF core\u2010shell structures and establishes a versatile nanoplatform for deep glycomics analysis in complex biological fluids.\n                  <\/jats:p>","DOI":"10.1002\/smll.75368","type":"journal-article","created":{"date-parts":[[2026,8,21]],"date-time":"2026-08-21T11:06:48Z","timestamp":1787310408000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Hierarchically Porous MOF Shell Nanoengineered on Magnetic Cores as a Nanoplatform Towards Serum Glycopeptide Decoding"],"prefix":"10.1002","volume":"22","author":[{"given":"Yiwen","family":"Lin","sequence":"first","affiliation":[{"name":"Department of Chemistry Fudan University  Shanghai 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