A method using reversed-phase ion-pair high-performance liquid chromatography with electrochemical detection for the simultaneous determination of biogenic amines and metabolites has been developed. Two mobile phases one free of involatile substances have been compared for the separation of vanillylmandelic acid, 3,4-dihydroxy-phenylalanine, 3-methoxy-4-hydroxyphenylglycol, 3,4-dihydroxyphenylacetic acid, norepinephrine, 5-hydrozyindoleacetic acid, epinephrine, homovanillic acid, dopamine, serotonin, and 3-methoxytyramine. The present method can be applied to the analysis of brain, cerebrospinal fluid and plasma. Minimal sample preparation for brain and cerebrospinal fluid is required before injection into the liquid chromatograph. Molecular sieve chromatography and organic extraction is used for plasma cleanup for homovanillic acid determination. The procedure offers an attractive possibility for routine analysis of biogenic amines and their metabolites.