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Here, we report QC4A\u20108C, a single compartmentalized supramolecular platform that simultaneously addresses these limitations. QC4A\u20108C is an amphiphilic quaternary ammonium calix[4]arene with orthogonally functionalized upper and lower rims. The cationic cavity selectively encapsulates luminol, induces a p\n                    <jats:italic>K<\/jats:italic>\n                    a shift, and converts luminol into a glow\u2010type emitter at near\u2010physiological pH. In parallel, the hydrophobic lower rim self\u2010assembles into nanoaggregates that compartmentalize fluorescent acceptors (DTBT, MCCH, DCI) in nanometer proximity, enabling sequential chemiluminescence resonance energy transfer (CRET) with high efficiency and red\u2010shifted emission (650\u2013700\u00a0nm). As a result, tissue penetration and emission lifetime are substantially extended, and in a lipopolysaccharide\u2010induced peritonitis model, QC4A\u20108C delivers pronounced signal enhancement over free luminol. This work validates macrocyclic host\u2013guest chemistry as a programmable route to integrate CL amplification with optical spectral engineering for diagnostic imaging.\n                  <\/jats:p>","DOI":"10.1002\/smll.75000","type":"journal-article","created":{"date-parts":[[2026,8,4]],"date-time":"2026-08-04T10:35:05Z","timestamp":1785839705000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Compartmentalized Amplification and Spectral Engineering of Luminol Chemiluminescence via Host\u2013Guest Cavity Binding and Amphiphilic Self\u2010Assembly"],"prefix":"10.1002","volume":"22","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-6143-6284","authenticated-orcid":false,"given":"Jie","family":"Gao","sequence":"first","affiliation":[{"name":"School of Pharmacy Guizhou International Science &amp; Technology Cooperation Base of Medical Optical Theranostics Research Key Laboratory of Basic Pharmacology of Ministry of Education and Joint International Research Laboratory of Ethnomedicine of Ministry of Education New Drug Discovery and Evaluation Center for International Cooperation and Disciplinary Innovation (\u201c111 Center\u201d) Zunyi Medical University  Zunyi Guizhou People's Republic of China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hongchao","family":"Wang","sequence":"additional","affiliation":[{"name":"School of Pharmacy Guizhou International Science &amp; Technology Cooperation Base of Medical Optical Theranostics Research Key Laboratory of Basic Pharmacology of Ministry of Education and Joint International Research Laboratory of Ethnomedicine of Ministry of Education New Drug Discovery and Evaluation Center for International Cooperation and Disciplinary Innovation (\u201c111 Center\u201d) Zunyi Medical University  Zunyi Guizhou People's Republic of 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Ministry of Education New Drug Discovery and Evaluation Center for International Cooperation and Disciplinary Innovation (\u201c111 Center\u201d) Zunyi Medical University  Zunyi Guizhou People's Republic of China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Meng\u2010meng","family":"Chen","sequence":"additional","affiliation":[{"name":"School of Pharmacy Guizhou International Science &amp; Technology Cooperation Base of Medical Optical Theranostics Research Key Laboratory of Basic Pharmacology of Ministry of Education and Joint International Research Laboratory of Ethnomedicine of Ministry of Education New Drug Discovery and Evaluation Center for International Cooperation and Disciplinary Innovation (\u201c111 Center\u201d) Zunyi Medical University  Zunyi Guizhou People's Republic of China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yumei","family":"Wu","sequence":"additional","affiliation":[{"name":"School of Pharmacy Guizhou International Science &amp; Technology Cooperation Base of Medical Optical Theranostics Research Key Laboratory of Basic Pharmacology of Ministry of Education and Joint International Research Laboratory of Ethnomedicine of Ministry of Education New Drug Discovery and Evaluation Center for International Cooperation and Disciplinary Innovation (\u201c111 Center\u201d) Zunyi Medical University  Zunyi Guizhou People's Republic of China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zhe","family":"Zheng","sequence":"additional","affiliation":[{"name":"College of Chemistry Tianjin Key Laboratory of Structure and Performance for Functional Molecules Tianjin Normal University  Tianjin People's Republic of China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7450-4867","authenticated-orcid":false,"given":"Chunju","family":"Li","sequence":"additional","affiliation":[{"name":"College of Chemistry Tianjin Key Laboratory of Structure and Performance for Functional Molecules Tianjin Normal University  Tianjin People's Republic of China"},{"name":"Academy of Interdisciplinary Studies on Intelligent Molecules Tianjin Normal University  Tianjin People's Republic of China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5354-769X","authenticated-orcid":false,"given":"Zeli","family":"Yuan","sequence":"additional","affiliation":[{"name":"School of Pharmacy Guizhou International Science &amp; Technology Cooperation Base of Medical Optical Theranostics Research Key Laboratory of Basic Pharmacology of Ministry of Education and Joint International Research Laboratory of Ethnomedicine of Ministry of Education New Drug Discovery and Evaluation Center for International Cooperation and Disciplinary Innovation (\u201c111 Center\u201d) Zunyi Medical University  Zunyi Guizhou People's Republic of 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