A new ultrasensitive and ultrafast Al(III) metal−organicframework (MOF)-based probe (1) was constructed to detect Pd 2+ ions. Extremely selective recognition of Pd 2+ ion was demonstrated by the guest-free compound 1 (called 1′) using a fluorescence signal. The quenching in the fluorescence signal was observed due to the weak interaction between the linker alkyne−π bond and Pd 2+ . The mechanism of isophthalic alkyne−π and Pd 2+ interaction was systematically examined with the help of isothermal titration calorimetry (ITC), Xray photoelectron spectroscopy (XPS), and UV−vis spectroscopy. The response time of the MOF for sensing of Pd 2+ was 30 s, which is the lowest response time for MOF-based Pd 2+ sensing to date, with an ultralow detection limit (102 nM) and Stern−Volmer constant (4.39 × 10 3 M −1 ), evidencing the outstanding ability to sense Pd 2+ ion by this probe. The Pd 2+ detection limit falls among the lowest values. Activated MOF (1′) also showed considerable recyclability up to five steps with a constant sensing ability. In different water resources (Milli-Q water, lake water, river water, and tap water), the probe also showed excellent sensing ability. A paper-strip device was developed for the applicability of our material for the real field sensing application of Pd 2+ . The relevance of 1′ is not only up to Pd 2+ , but it could also sense palladium in other possible oxidation states.