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Here, it is aimed to introduce a new detoxification methodology for macromolecular biotoxin through complexation by a very large macrocycle. A 25\u2010<jats:italic>mer<\/jats:italic> peptide isolated from <jats:italic>Lycosa erythrognatha<\/jats:italic> spider venom (LyeTxI) is selected as the model macromolecular biotoxin. Quaterphen[4]arene, with a side length of \u22481.6\u00a0nm, has a sufficient cavity to bind LyeTxI. Hence, the water\u2010soluble derivative of Quaterphen[4]arene (H) is designed and synthesized. <jats:bold>H<\/jats:bold> exhibits an overall host\u2013guest complexation toward LyeTxI, resulting in a considerably high association constant of (7.01\u00a0\u00b1\u00a00.18)\u00a0\u00d7\u00a010<jats:sup>7<\/jats:sup>\u00a0<jats:sc>m<\/jats:sc><jats:sup>\u22121<\/jats:sup>. This encapsulation of peptide is interesting as traditional macrocycles can only engulf the amino acid residues of peptides due to their limited cavity size. In vitro assay verifies that complexation by <jats:bold>H<\/jats:bold> inhibits the interactions of LyeTxI with cell membranes, thereby reducing its cytotoxicity, suppressing hemolysis, and decreasing the release of lactate dehydrogenase. Notably, the intravenous administration of <jats:bold>H<\/jats:bold> has a significant therapeutic effect on LyeTxI\u2010poisoned mice, alleviating inflammation and tissue damage, and markedly improving the survival rate from 10% to 80%. An efficient and potentially versatile approach is provided to detoxify macromolecular biotoxins, with giant macrocycle serving as an antidote.<\/jats:p>","DOI":"10.1002\/adhm.202200270","type":"journal-article","created":{"date-parts":[[2022,5,11]],"date-time":"2022-05-11T06:41:18Z","timestamp":1652251278000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":26,"title":["Supramolecular Detoxification of Macromolecular Biotoxin through the Complexation by a Large\u2010Sized Macrocycle"],"prefix":"10.1002","volume":"11","author":[{"given":"Liang","family":"Zhao","sequence":"first","affiliation":[{"name":"Center for Supramolecular Chemistry and Catalysis Department of Chemistry Shanghai University  Shanghai 200444 P. R. China"},{"name":"State Key Laboratory of Toxicology and Medical Countermeasures Beijing Institute of Pharmacology and Toxicology  Beijing 100850 P. R. 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