Abstract: Pre-separation and concentration of polyamines in urine were accomplished with an ion exchange column.The enriched polyamines were then acylated.The optimum conditions for ion-exchange were determined and the acylation effect of three acylating agents was compared.The derived product was analyzed by capillary gas chromatography.The contents of polyamines in urine were thus determinned. The results obtained show that the quantity of polyamines in urine of cancer patients is higher than that of normal person.