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To overcome these challenges, we developed an innovative therapeutic formulation that integrates targeted chemotherapy and phototherapy within a single platform using gold nanoparticles (AuNPs). This novel nanoconjugate, designated as <jats:bold>Dox\u2010Fe@FA\u2010AuNPs<\/jats:bold>, is co\u2010functionalized with folic acid, doxorubicin, and an iron(III)\u2010phenolate\/carboxylate complex, enabling cancer\u2010specific drug activation. Here, we report the synthesis, characterization, and comprehensive physico\u2010chemical and biological evaluations of <jats:bold>Dox\u2010Fe@FA\u2010AuNPs<\/jats:bold>. The nanoconjugate exhibited excellent solubility, stability, and enhanced cellular uptake in folate receptor\u2010positive cancer cells. The nanoconjugate was potently cytotoxic against HeLa and MDA\u2010MB\u2010231 cancer cells (HeLa: 105.5\u00b116.52\u2005\u03bcg\u2009mL<jats:sup>\u22121<\/jats:sup>; MDA\u2010MB\u2010231: 112.0\u00b112.31\u2005\u03bcg\u2009mL<jats:sup>\u22121<\/jats:sup>; MDA\u2010MB\u2010231 (3D): 156.31\u00b119.35\u2005\u03bcg\u2009mL<jats:sup>\u22121<\/jats:sup>) while less cytotoxic to the folate(\u2212) cancer cells (MCF\u20107, A549 and HepG2). The cytotoxicity was attributed to the pH\u2010dependent release of doxorubicin, which preferentially occurs in the acidic tumor microenvironment. Additionally, under red light irradiation, the nanoconjugate generated ROS, inducing caspase\u20103\/7\u2010dependent apoptosis with a photo\u2010index (PI) &gt;50, and inhibited cancer cell migration. Our findings underscore the potential of <jats:bold>Dox\u2010Fe@FA\u2010AuNPs<\/jats:bold> as a highly effective and sustainable platform for targeted chemo\u2010phototherapy.<\/jats:p>","DOI":"10.1002\/asia.202400616","type":"journal-article","created":{"date-parts":[[2024,6,26]],"date-time":"2024-06-26T10:15:00Z","timestamp":1719396900000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":5,"title":["Targeted Chemo\u2010Phototherapy in Red Light with Novel Doxorubicin and Iron(III) Complex\u2010Functionalized Gold Nanoconjugate (Dox\u2010Fe@FA\u2010AuNPs)"],"prefix":"10.1002","volume":"19","author":[{"given":"Maynak","family":"Pal","sequence":"first","affiliation":[{"name":"Department of Chemistry National Institute of Technology Manipur  Langol 795004 Imphal West, Manipur"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Arpan","family":"Bera","sequence":"additional","affiliation":[{"name":"Department of 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