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Doxorubicin (Dox)-loaded gold nanoparticles (Dox@AuNPs) were developed and evaluated for enhanced anticancer activity. The nanocomposites exhibited spherical morphology (13\u2009\u00b1\u20093\u00a0nm) with a loading efficiency of 52%. In vitro, Dox@AuNPs reduced the IC\u2085\u2080 by approximately 50% compared to free Dox in MCF-7 cells. In vivo, treatment significantly suppressed tumor growth and increased median survival (62 days) relative to free Dox (52 days). In addition to conventional efficacy evaluation, Fourier transform infrared (FTIR) spectroscopy was applied to analyze biochemical changes in tumor tissues. Distinct alterations in protein, lipid, and nucleic acid-associated bands were observed, with treated tissues showing partial spectral shifts toward normal profiles. These findings suggest that FTIR may provide additional insight into tissue-level biochemical responses following treatment. 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