Overdose of procaine may lead to many health problems. However, highly sensitive detection of procaine has always been a challenge. Electrochemical sensor is of great significance in the field of life and health due to its high sensitivity, low cost and compatibility with portable technology. In this work, a sensor based on diamond/graphite hybrid with a molecular imprinting membrane was developed. The sp 3 -bonded diamond and sp 2 -bonded graphite have good mechanical properties and wide potential window. The molecular imprinting membrane can be immobilized on the diamond/graphite surface for selective determination of procaine. The optimized conditions allowed the sensor to detect the procaine concentration linearly in the range of 4×10 -8 -2.5 ×10 -5 M. The limits of detection were calculated to be 1.5×10 -8 M.