Indium, copper, and mercury are important raw materials in the electronics industry and often coexist in factory wastewater. Therefore, the development of a highly sensitive and selective method for the simultaneous detection of these heavy metal ions is of great significance for water quality monitoring and environmental protection. Herein, we report a NH 2 -MIL-53 fluorescent probe for the simultaneous detection of trace In 3+ , Cu 2+ , and Hg 2+ in water. After a low-temperature NH 3 plasma tailoring treatment for grafting electron-donor amine groups, the obtained NH 2 -MIL-53-M exhibited enhanced fluorescence emission intensity (∼6 times) coupled with selective adsorption of In 3+ , Cu 2+ , and Hg 2+ . This quenched the NH 2 -MIL-53-M fluorescence and allowed to significantly increase the selectivity and sensitivity for detection of In 3+ , Cu 2+ , and Hg 2+ . The fluorescence quenching constant (K sv ) values were 2.23 × 10 5 , 1.00 × 10 5 , and 2.74 × 10 4 M −1 , while the limit of detection (LODs) values were 0.06, 0.14, and 0.53 μM, for In 3+ , Cu 2+ , and Hg 2+ , respectively. The concentrations of In 3+ , Cu 2+ , and Hg 2+ in real environmental samples could be determined by addition of appropriate masking agents, and the recoveries were within the range of 94−110%. This study not only supplied a strategy for constructing a highly sensitive and selective fluorescent probe but also established a platform for simultaneous detection of multiple heavy metal ions in water.