In this study, the composite material that made up polyglycine/3d-4f hybrid-metallic cyano-bridged mixed coordination polymers (CyMCP) was successfully decorated onto a glassy carbon rotating disk electrode (GC RDE) using electrodeposition. The voltammetric behavior of NADH showed typical direct electrooxidation characteristics on the modified GC electrode. Our polyglycine/CyMCP-modified GC RDE was able to measure the apparent heterogeneous electron transfer rate constant of NADH during its direct electrooxidation by preventing fouling effects on the working electrode, which would generally cause a decrease in the oxidative peak current of NADH. In addition, differential pulse voltammetry provided a large linear range between the oxidative peak current and the concentration of NADH from 2-1500 mu M at the polyglycine/CyMCP/GC electrode. Finally, the apparent heterogeneous electron transfer rate constant (k(s)(NADH)) of NADH was determined to be 1.73 x 10(-2) cm.s(-1) using the polyglycine/CyMCP-modified GC RDE. (C) The Author(s) 2015. Published by ECS. All rights reserved.