The analysis of biogenic amine neurotransmitters (adrenaline, noradrenaline, dopamine, serotonin) and their metabolites (metanephrine, normetanephrine, 3,4-dihydroxyphenylacetic acid, vanillylmandelic acid, homovanillic acid, 5-hydroxyindoleacetic acid, 3,4-dihydroxyphenylglycol, 3-methoxy-4-hydroxyphenylglycol, 3-methoxytyramine) in body fluids may provide valuable information important in the diagnosis of the sympathoadrenomedullary system disturbances. An HPLC-FL/ED system using two Chromolith RP-18e columns and a mixture of acetate buffer (pH=4.66) and methanol (973%, v/v) as the mobile phase was developed for the separation and determination of these compounds. Adrenaline, noradrenaline, dopamine and their synthetic analogs: dobutamine and isoproterenol, used in the treatment of clinical shock, were analyzed in urine of post-operative cardiosurgical patients and in urine of healthy controls. The extraction and pre-concentration step was performed on aluminium oxide SPE cartridges. Both detection techniques agreed well in final concentrations. Within-day coefficients of variation were below 2.3% and between-day coefficients of variation did not exceed 5%. The developed HPLC method is easy and reliable and could have a positive effect on the safety of severely ill patients treated with catecholamines and their synthetic analogues.