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Convenient, rapid, highly sensitive and on-site iron determination is important for environmental safety and human health. We developed a sensing system for the detection of Fe(III) in water based on 7-mercapto-4-methylcoumarine (MMC)-stabilized silver-coated gold nanostars (GNS@Ag@MMC), exploiting a redox reaction between the Fe(III) cation and the silver shell of the nanoparticles, which causes a severe transformation of the nanomaterial structure, reverting it to pristine GNSs. This system works by simultaneously monitoring changes in the Localized Surface Plasmon Resonance (LSPR) and Surface-Enhanced Raman Spectroscopy (SERS) spectra as a function of added Fe(III). The proposed sensing system is able to detect the Fe(III) cation in the 1.0 × 10⁻⁵–1.5 × 10⁻⁴ M range, and its selectivity of the GNS@Ag@MMC sensor toward iron has been verified monitoring the LSPR and the SERS response to other cations with a clear selectivity toward Fe(III).