A novel dual-emission responsive near-infrared fluorescent probe (2-OH-TCF-NBD) for the detection and discrimination of Cys/Hcy, GSH/H2S 2 S was developed on the basis of the conjugation of a tricyanofuran-based fluorophore (2-OH-TCF) and 4-chloro-7-nitrobenzofurazan (NBD-Cl). When the probe was added to the Cys/ Hcy solution, it resulted in significant fluorescence enhancement at both 527 and 630 nm, while GSH/H2S 2 S induced major fluorescence emission only at 630 nm. The detection limits for Cys, Hcy, GSH, and H2S 2 S were determined to be 0.029, 0.020, 0.29, and 0.20 mu M, respectively. Furthermore, the probe demonstrated some merits including easy preparation, rapid response time, and good anti-interference ability. The possible response mechanism was also proposed and validated by HPLC analysis of the reaction process. Therefore, the probe can be a potential tool for discriminating the detection of Cys/Hcy and GSH/H2S 2 S under physiological conditions.