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However, biofluids present several challenges to biosensor sensing and stability on account of their complex composition and dynamic nature. Surface\u2010enhanced Raman spectroscopy (SERS) offers ultra\u2010high sensitivity, non\u2010destructive, real\u2010time monitoring, and non\u2010invasive detection, ideal for sensing in complex media. Plasmonic gold nanoparticle (AuNP) SERS\u2010active assemblies have been widely explored owning to their biocompatibility and tunable sensitivity based on AuNP morphology. Here, we employ thiolated poly(ethylene glycol) (PEG\u2010SH) to produce kinetically trapped metastable AuNP:cucurbit[7]uril (CB[7]) aggregates containing robust nanogaps (ca. 1\u00a0nm), which have previously displayed strong, reproducible SERS signals at low concentrations. The AuNP:CB[7]:PEG aggregates maintain strong SERS\u2010activity, demonstrating low concentration detection of a model Raman reporter and a bioanalyte in a range of biofluids. Moreover, the aggregates are highly tunable through facile modification of the PEG\u2010SH chain length and grafting density and possess an encoded disassembly mechanism within their design highlighting the potential application of these aggregates for non\u2010invasive in vivo long\u2010term monitoring alongside future customized SERS biosensing\u00a0applications.<\/jats:p>","DOI":"10.1002\/chem.202500915","type":"journal-article","created":{"date-parts":[[2025,4,17]],"date-time":"2025-04-17T09:37:21Z","timestamp":1744882641000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":6,"title":["Kinetically Arrested SERS\u2010Active Aggregates for Biosensing"],"prefix":"10.1002","volume":"31","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-2368-2302","authenticated-orcid":false,"given":"Natalie S.","family":"Potter","sequence":"first","affiliation":[{"name":"Melville Laboratory for Polymer Synthesis Yusuf Hamied Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Kamil","family":"Soko\u0142owski","sequence":"additional","affiliation":[{"name":"Melville Laboratory for Polymer Synthesis Yusuf Hamied Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5446-5346","authenticated-orcid":false,"given":"Renata Lang","family":"Sala","sequence":"additional","affiliation":[{"name":"Melville Laboratory for Polymer Synthesis Yusuf Hamied Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5048-2683","authenticated-orcid":false,"given":"Jade A.","family":"McCune","sequence":"additional","affiliation":[{"name":"Melville Laboratory for Polymer Synthesis Yusuf Hamied Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8032-7166","authenticated-orcid":false,"given":"Oren A.","family":"Scherman","sequence":"additional","affiliation":[{"name":"Melville Laboratory for Polymer Synthesis Yusuf Hamied Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UK"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2025,6,17]]},"reference":[{"key":"e_1_2_8_1_1","doi-asserted-by":"publisher","DOI":"10.1002\/adma.201400203"},{"key":"e_1_2_8_2_1","doi-asserted-by":"publisher","DOI":"10.1021\/cr300213b"},{"key":"e_1_2_8_3_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.chemrev.6b00196"},{"key":"e_1_2_8_4_1","doi-asserted-by":"publisher","DOI":"10.1126\/science.1125124"},{"key":"e_1_2_8_5_1","doi-asserted-by":"publisher","DOI":"10.1126\/science.aba8653"},{"key":"e_1_2_8_6_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.chemmater.5b03821"},{"key":"e_1_2_8_7_1","doi-asserted-by":"publisher","DOI":"10.1002\/(SICI)1521-4095(199910)11:14<1202::AID-ADMA1202>3.0.CO;2-H"},{"key":"e_1_2_8_8_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.201209336"},{"key":"e_1_2_8_9_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41563-019-0549-3"},{"key":"e_1_2_8_10_1","doi-asserted-by":"publisher","DOI":"10.1038\/nmat4526"},{"key":"e_1_2_8_11_1","doi-asserted-by":"publisher","DOI":"10.1038\/nmat3867"},{"key":"e_1_2_8_12_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.chemmater.9b02216"},{"key":"e_1_2_8_13_1","doi-asserted-by":"publisher","DOI":"10.1038\/nmat3509"},{"key":"e_1_2_8_14_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41565-021-00949-6"},{"key":"e_1_2_8_15_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41565-020-0643-3"},{"key":"e_1_2_8_16_1","doi-asserted-by":"publisher","DOI":"10.1021\/jacs.9b01883"},{"key":"e_1_2_8_17_1","doi-asserted-by":"publisher","DOI":"10.1039\/b925051d"},{"key":"e_1_2_8_18_1","doi-asserted-by":"publisher","DOI":"10.1038\/srep06785"},{"key":"e_1_2_8_19_1","author":"Taylor R. 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