Steroid metabolites in carp (Cyprinus carpio) urine were hydrolyzed with β-glucuronidase and by solvolysis (ethylacetate-1 N H_2SO_4) . The liberated steroids were extracted with ethylacetate, converted to methoxime-trimethylsilyl derivatives, and subjected to gas chromatographic (GC) analysis. The GC separations were carried out on 1 % OV-1 and 2 % QF-1 columns, and the retention data (MU values) of carp urinary steroids ( I -XIII) were compared with those of reference steroids identically treated with the above procedures (Table 1). The structures of the compounds I -X were also confirmed by GC-Mass spectrometry. The results showed the presence of androsterone, etiocholanolone, DHEA, androstenediol, pregnanediol, pregnanetriol, cholesterol, THE, THF, cortolone, β-cortolone, cortol and β-cortol in the urine of carp.