A method is described which extends a high performance liquid chromatographic assay for urinary catecholamines to the assay of urinary metanephrines. The amines are separated from urine after acid hydrolysis of conjugates by ion-exchange chromatography, and then further purified by solvent extraction. The final extracts are suitable for direct HPLC assay using the endogenous fluorescence of the amines for detection. Twenty-four hour excretion of the amines in 35 hospital in-patients was found to be (mean and range: 169 micrograms/24 h normetanephrine (39-423), 102 micrograms/24 h metanephrine (19-290) and 138 micrograms/24 h 3-methoxytyramine (32-234)).

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