The synthesis of lignin-based graphene quantum dots (GQDs) with excellent fluorescence stability, quantum yield, and biocompatibility for sensitive and selective detection of Fe and ascorbic acid (AA) has remained a challenging endeavor. Using an acidolysis process with 17.5% nitric acid followed by hydrothermal treatment at 200 °C, this study provided an improved synthesis route for the production of high-quality GQDs from alkali lignin. The nitrogen-doped GQDs exhibit remarkable fluorescence stability under a wide range of pH (3-10), duration (1-12 h), and [NaCl] (0-1000 mM) conditions, and have a high quantum yield of 28%. The GQDs or GQDs/Fe sensing systems ([GQDs] at 50 mg L, [Fe] at 500 μmol L, and UV excitation at 370 nm) for fluorescence sensing of Fe or AA have excellent sensitivity, selectivity, and reproducibility. For Fe and AA, the limit of detection is 1.49 and 1.62 μmol L, respectively. Mechanism investigation shows that photoluminescence quenching is caused by the formation of GQDs-Fe complexes, whereas fluorescence recovery is due to Fe reduction by AA.
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