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Herein, we present a plasmonic coacervate platform that spontaneously sequesters polystyrene (PS) MNPs from water while facilitating surface\u2010enhanced Raman scattering (SERS) detection. Coacervate microdroplets, formed through the liquid\u2013liquid phase separation (LLPS) of cationic poly(diallyldimethylammonium chloride) and anionic adenosine triphosphate, exhibit a positive surface charge and a hydrophobic interior, enabling capture of nanoscale or microscale negatively charged PS MNPs with enrichment rates of 99.4% and 91.1%. The co\u2010encapsulation of silver nanoparticles (AgNPs) generates three\u2010dimensional droplet\u2010confined SERS hotspot networks, resulting in an enhancement factor of 2.72 \u00d7 10\n                    <jats:sup>9<\/jats:sup>\n                    , excellent uniformity, and minimum detectable concentration of 1 and 10\u00a0ng\/mL for nano\u2010 and micro\u2010scale PS, demonstrating strong linear correlations. This platform achieves recoveries ranging from 87% to 108% for PS MNPs spiked into filtered tap and river water and successfully detects PS MNPs released from commercial plastic cups and expanded polystyrene containers under simulated daily use. Our work establishes a simple, rapid, and sensitive strategy that integrates spontaneous analyte sequestration with plasmonic amplification, thus offering a new avenue for monitoring MNPs and assessing the safety of food\u2010contact materials.\n                  <\/jats:p>","DOI":"10.1002\/adma.75459","type":"journal-article","created":{"date-parts":[[2026,10,21]],"date-time":"2026-10-21T11:21:21Z","timestamp":1792581681000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Spontaneous Capture, Enrichment, and SERS Sensing of Polystyrene Micro\/Nanoplastics Enabled by Condensed Plasmonic Coacervate Droplets"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0009-0008-2436-4139","authenticated-orcid":false,"given":"Junbo","family":"Li","sequence":"first","affiliation":[{"name":"College of Chemistry Chemical Engineering and Resource Utilization Northeast Forestry University  Harbin China"},{"name":"State 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