topologies, respectively. Ratiometric fluorescence responses of Ni-MOFs toward various per-/polyfluoroalkyl substances (PFASs) in aqueous media were investigated by fluorescence sensing assays. The sensing performance of MOF1 and MOF2 toward perfluorooctanoic acid (PFOA) and trifluoroacetic acid (TFA) revealed that Ni-MOFs have low detection limits and high immunity to interference as well as excellent recycling stability. Mechanism investigations show that MOF1's response is mainly due to PFOA affecting the coordination environment of Ni(II), whereas that of MOF2 is caused by interactions between the TFA and the framework resulting in a proportional fluorescence response to the analytes.