The catalytic activity of a carbon fiber microelectrode modified with cobalt phthalocyanine (CoPc-ME) for the detection of nitric oxide in the presence of possible interfering molecules (dopamine and serotonin) is examined. A linear plot is observed for the variation of the catalytic currents with NO concentration in the presence of excess dopamine and serotonin, showing that NO may be determined in the presence of these molecules. However, oxidation currents due to serotonin were found to decrease with increase in NO concentration. The CoPc-ME could also detect NO added to blood or its components, the oxidation currents for NO, however, decreased rapidly with time. The decrease in currents was slower in blood serum, followed by whole blood, with a faster decrease being observed in blood plasma.