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Pyridoxal 5′-phosphate (PLP), a biologically important coenzyme, participates in several enzymatic reactions, and its marginal deficiency in the human body can cause cardiovascular disease. However, the excess accumulation of the non-essential Al3+ metal ion in the human body can also cause serious health problems. Therefore, there is significant interest in the detection and monitoring of both PLP and Al3+. This paper introduced a red-emitting dual-ligand co-functionalized copper nanoclusters β-CD-GSH-CuNCs for the simultaneous detection of PLP and Al3+. The capped β-cyclodextrin (β-CD) in β-CD-GSH-CuNCs selectively recognizes PLP by forming a host–guest inclusion complex that caused fluorescence quenching at 625 nm with the formation of an emission band at 488 nm. The ratiometric fluorescence from β-CD-GSH-CuNCs allowed to detect PLP down to 5.29 μM. Further, the in situ-generated nano-assembly β-CD-GSH-CuNCs@PLP showed a selective turn-on fluorescent response for Al3+. The complexation-induced aggregation of nano-assembly resulted in strong fluorescence enhancement at 451 nm that allowed to detect Al3+ down to 0.187 μM. The analytical utility of β-CD-GSH-CuNCs@PLP was validated as a nanoprobe by monitoring Al3+ concentrations in real environmental water samples.

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