In this work, we present a facile, green synthetic strategy for the preparation of bismuth@carbon nanostructures (Bi@C) using glucose as carbon source via a one-pot template-free hydrothermal approach. Inspiringly, Bi@C exhibits good conductivity of organic carbon, which is very important for electrode construction. Further, to obtain more active -COOH groups and better monodispersity, Bi@C was decorated with 3,4,9,10-perylenetetracarboxylic acid (PTCA). The interesting Bi@C-PTCA nanostructures serve as a sensing platform and show well-separated oxidation peaks and enhanced peak currents for selective determination of ascorbic acid (AA), dopamine (DA) and uric acid (UA). Under the optimized experimental condition, the linear responses for simultaneous detection of AA, DA and UA are 1.0-119 mu M, 0.2-87.2 mu M and 0.1-119.1 mu M, and the detection limits are 0.27 mu M, 0.06 mu M and 0.03 mu M (S/N = 3), respectively. Importantly, the fabricated electrochemical sensor exhibits long-term sensing stability, behaves as a good anti-interference response, and has promising applications for the determination of multi-analytes in human urine and serum samples. (C) 2017 The Electrochemical Society. All rights reserved.