A capillary gas-chromatographic method with nitrogen-phosphorus detection is used to determine simultaneously urinary 1,3-diaminopropane, monoacetyl-1,3-diaminopropane, putrescine, monoacetylputrescine, cadaverine, monoacetylcadaverine, spermidine, N1-acetylspermidine, N beta-acetylspermidine, spermine, N1-acetylspermine, isoputreanine, N-(3-aminopropyl)pyrrolidin-2-one, and putreanine. The compounds are isolated by adsorption onto silica and converted into their methyl-heptafluorobutyryl derivatives. We give quality-control data and age-dependent "normal" values for urinary excretion of these analytes from 51 apparently healthy control subjects. Normal values for 31 adults are compared with those reported in the literature. Monoacetyl-1,3-diaminopropane and N1-acetylspermine are identified by mass fragmentography. We applied the method to monitor chemotherapeutic treatment of a patient with advanced non-Hodgkin's lymphoma; we identified by mass spectrometry N1,N12-diacetylspermine in this patient's urine.