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A series of bishydrazide compounds have been developed for selective turn-on detection of Al³⁺ cation, based on metal chelation-enhanced fluorescence (CHEF) effects that inhibit the nonradiative PET and ESIPT processes. In aqueous solution, Al³⁺ selectively induces strong fluorescence of these compounds with large Stokes shifts up to ∼133 nm and emission colors varying from blue to orange. In the solid phase, both Al³⁺ and Zn²⁺ give apparent fluorescence which is simultaneously detected based on chromatographic separation.