We monitored electrooxidation of noradrenaline and α-melanocyte stimulating hormone (α-MSH) at a carbon-fibre microelectrode (CFME). The solution of noradrenaline (1 mM) or α-MSH (1 mM) was applied by a pressure pulse (2 s) from a micropipette to a voltage-clamped (850 mV) CFME immersed into bathing solution of an inverted microscope chamber. The distance between the CFME and micropipette was 2 to 12 μm. The maximal currents recorded for these two agents were 8.0 ± 0.5 pA (N = 9) and 3.0 ± 1.1 pA (N = 9), respectively. Pressure application of control solution did not affect the measured current. The noradrenaline-evoked anodic current was characterized by a monotonic increase that attained the maximum at the end of the pressure pulse. In contrast, the time-course of the α-MSH-evoked current was biphasic. The maximum amplitude of this current was attained in 0.59 ± 0.15 s (N = 9) and then it declined with a time constant of 7.5 ± 4.0 s (N = 9) until the pressure pulse was terminated. We explain this phenomenon to be due to an interaction between the peptide oxidation products and the CFME which results in its desensitization.