An easy and effective strategy for synthesizing a ratiometric fluorescent nanosensor has been demonstrated in this work. Novel fluorescent BSA-AuNPs@Tb-AMP (BSA, bovine serum albumin; AMP, adenosine 5'-monophosphate; AuNPs, Au nanoparticles) metal-organic framework (MOF) nanostructures were synthesized by encapsulating BSA-AuNPs into Tb-AMP MOFs for the detection of 2,6-pyridinedicarboxylic acid (DPA) and Hg . DPA could strongly co-ordinate with Tb to replace water molecules from the Tb center and accordingly enhanced the fluorescence of Tb-AMP MOFs. The fluorescence of BSA-AuNPs at 405 nm remained constant. While the fluorescence of BSA-AuNPs at 635 nm was quenched after Hg was added, the fluorescence of Tb-AMP MOFs remained constant. Accordingly, a ratiometric fluorescence nanosensor was constructed for detection of DPA and Hg . The ratiometric nanosensor exhibited good selectivity to DPA over other substances. The F /F linearly increased with increase of DPA concentration in the range of 50 nM to 10 μM with a detection limit as low as 17.4 nM. F /F increased linearly with increase of Hg concentration ranging from 50 nM to 1 μM with a detection limit as low as 20.9 nM. Additionally, the nanosensor could be successfully applied for the determination of DPA and Hg in running water.