The monoamine oxidase A metabolite of noradrenaline, 3,4-dihydroxyphenylglycolaldehyde, is the precursor of 3,4-dihydroxymandelic acid, and 3,4-dihydroxyphenylglycol, metabolites of noradrenaline. Owing to difficulties in purifying this aldehyde, it has not been previously characterized or identified in biological sources. This paper describes an enzymatic synthesis, purification, and characterization of 3,4-dihydroxyphenylglycolaldehyde. The aldehyde metabolite is identified in postmortem human brain using highperformance liquid chromatography and electrochemical detection. We estimate the concentration in human hippocampus to be 0.164 ± 0.05 nmol/g. The importance of this aldehyde metabolite of noradrenaline is discussed.