| Summary: | Ethyl-thioglycolate-modified Fe<sub>3</sub>O<sub>4</sub>@ZnS nanoparticles (Fe<sub>3</sub>O<sub>4</sub>@ZnS-SH) were successfully prepared using a simple chemical precipitation method. The introduction of ethyl thioglycolate better regulated the surface distribution of ZnS, which can act as a recognition group and can cause a considerable quenching of the fluorescence intensity of the magnetic fluorescent nanoprobe, Fe<sub>3</sub>O<sub>4</sub>@ZnS-SH. Benefiting from stable fluorescence emission, the magnetic fluorescent nanoprobe showed a highly selective fluorescent response to Ag+ in the range of 0–400 μM, with a low detection limit of 0.20 μM. The magnetic fluorescent nanoprobe was used to determine the content of Ag<sup>+</sup> in real samples. A simple and environmentally friendly approach was proposed to simultaneously achieve the enrichment, detection, and separation of Ag<sup>+</sup> and the magnetic fluorescent nanoprobe from an aqueous solution. These results may lead to a wider range of application prospects of Fe<sub>3</sub>O<sub>4</sub> nanomaterials as base materials for fluorescence detection in the environment.
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