Abstract: Clopamide as a new diuretic was forbidden by IOC.A new reliable GC/MSD determination method of clopamide in human urine is described in this paper.Three methyled compounds are found and varieties of extraction procedures are compared.The basic extraction recovery is 94.5%. The excretion profile of clopamide in human urine has been investigated.Clopamide could be detected in human urine within 20 hours.