A sensitive spectrophotometric method for the determination of three kdetosteriod drugs is suggested. The method is based on oximation, separation and acid cleavage of their oximes followed by spectro-photometric measurement of the liberated hydroxylamine through oxidation and diazo coupling reactions. The method gave mean percent recoveries of 98.92 ± 0.58, 99.26 ± 0.96, and 99 10 ± 0.47 for progesterone, testosterone propionate and nandrolone phenyl propionate respectively in ampoules. Results were in good agreement with B.P. 1980 method.