Optimum conditions for the separation of 9-fluorenylmethyl chloroformate derivatized catecholamines by HPLC are described; three catecholamines (noradrenaline, adrenaline and dopamine) and an internal standard (epinine) were separated in less than 20 minutes under isocratic conditions. This method is 17 to 350 times more sensitive than electrochemical detection, depending on the test compounds. It has been applied to the analysis of catecholamines in urine. The sample was extracted by a metal-loaded silica prior to separation.