Using gas chromatography mass spectrometry following derivatization (N-trifluoroacetylation), 1-N-acetylspermidine was found to occur in normal human serum at a level of approximately 0.008--0.5 nmol ml(-1), i.e. about two orders of magnitude lower than the corresponding spermidine level. No evidence for the occurrence in serum of the isomeric 8-N-acetylspermidine was found. Mass spectra of authentic samples of trifluoroactylated 1-N- and 8-N-acetylspermidine are presented.