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Fmoc\u2010hPhe\u2010OH (<jats:bold>hF<\/jats:bold>) forms a hydrogel in 50\u00a0mM phosphate buffer (PB) of pH 7.4. Interestingly, <jats:bold>hF<\/jats:bold>\u2010based hydrogel shows syneresis behavior with controlled release of residual water from the hydrogel matrix. Moreover, this hydrogelator can form co\u2010assembled hydrogels with various dyes, including Congo Red and Rhodamine B; natural water samples, including natural mud water and sea water; and heavy metal ions aqueous solutions, including Cd<jats:sup>II<\/jats:sup>, Pb<jats:sup>II<\/jats:sup>, and Hg<jats:sup>II<\/jats:sup> separately in 50\u00a0mM PB of pH 7.4. Interestingly, after 2 to 3 hours for shake gel and 5\u20136 hours for nonshake gel, the released waters have been tested and it has been found that these co\u2010assembled hydrogels are capable of retaining almost all the contaminants within the shrink hydrogels matrix and releasing almost pure water along with the presence of hydrogel nanofibers. Syneresis is augmented to purify the contaminated water with dyes, mud, dissolved salts, and toxic heavy metal ions. These co\u2010assembled hydrogels, leading to distinct structural and functional changes, which have been characterized by using Fourier\u2010Transform Infrared Spectroscopy (FTIR), X\u2010ray Diffraction (XRD), and Field Emission Scanning Electron Microscopy (FE\u2010SEM), suggesting various supramolecular interactions including \u03c0\u2010\u03c0 stacking, hydrogen bonding, and electrostatic interactions are responsible for stable hydrogelations. The rheological study evaluates the hydrogel's mechanical and thixotropic properties and spectroscopic techniques, including UV\u2010visible spectroscopy and fluorescence spectroscopy, to monitor structural transition. This novel class of amino acid\u2010based hydrogel shows antibacterial activity against both Gram\u2010positive and Gram\u2010negative bacteria, likely through membrane\u2010disruptive mechanisms, and also shows promising antioxidant properties. The native <jats:bold>hF<\/jats:bold> hydrogel is biocompatible and shows anticancer activity toward the pancreatic cancer cell line. The research finding bestows the biomedically relevant hydrogel's potential use in green and sustainable environmental remediation.<\/jats:p>","DOI":"10.1002\/chem.202501895","type":"journal-article","created":{"date-parts":[[2025,9,11]],"date-time":"2025-09-11T06:12:49Z","timestamp":1757571169000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":7,"title":["An Amino Acid\u2010Based Self\u2010Shrinking Supramolecular Bioactive Hydrogel \u2010 A Sustainable Platform for Wastewater Treatment and Water Purification"],"prefix":"10.1002","volume":"31","author":[{"given":"Swaraj Ganesh","family":"Gaonkar","sequence":"first","affiliation":[{"name":"Department of Chemistry Birla Institute of Technology and Science\u2010Pilani K K Birla Goa Campus  Zuarinagar Goa 403726 India"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Pandey Priya","family":"Arun","sequence":"additional","affiliation":[{"name":"Department of Medicinal Chemistry Institute of Medicinal Chemistry Institute of Medical Sciences Banaras Hindu University  Varanasi UP 221005 India"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"S. 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