Capillary gas chromatography and mass fragmentography was used to determine simultaneously 1,3-diaminopropane, putrescine, cadaverine, spermidine, spermine, isoputreanine and putreanine in cerebrospinal fluid. After addition of deuterium labelled analogs and acid hydrolysis, the compounds were isolated by adsorption onto silica and converted into their N-heptafluorobutyryl-methylesters. Quality control data and an application of the method are given. A patient harbouring an astrocytoma was monitored during chemotherapeutic treatment.