Abstract: | Although a variety of chemosensors as probes have been exploited for the detection of metal ions with high sensitivity and selectivity, the formed probe–metal complex was hardly suitable for separation, removal, and further recovery. This paper presents a method to detect and remove metal ions from aqueous solutions simultaneously by a fluorescence chemosensor and functional magnetic nanoparticles. A novel probe SRhB ‐Azo was synthesized based on rhodamine B (RhB ), maleic anhydride (MAH ), and azobenzene (Azo). SRhB ‐Azo showed high selectivity and sensitivity to Hg ions in aqueous solutions. Job's experiment showed the formation of a 1:2 stoichiometry complex between Hg2+ and SRhB ‐Azo. Moreover, β‐cyclodextrin (β‐CD )‐modified magnetic nanoparticles (CD‐MNPs ) were fabricated and used as host materials to form the inclusion complex CD–MNP and SRhB ‐Azo–Hg2+. Then, the SRhB ‐Azo‐Hg2+ complex could be removed by an external magnet, and subsequently recovered by UV ‐irradiation‐induced trans/cis isomerization of the Azo groups. The CD‐MNP s could be reused for nearly four times. Thus, the SRhB ‐Azo probe and CD‐MNP system has great potential application in sewage treatment. |