One hundred bovine thigh muscle samples were examined for detection of diethylstilboesterol residues using spectrophotometric technique. Extraction of the samples was carried out according to the method recommended by Umberger et al (1963). Diethylstilboesterol standard solution was prepared at concentration 20g/ml. For preparation of the working solution for spectrophotometric method 25m! from the prepared solution were mixed with 18% potassium monohydrogen phosphate solution (V/V). Finally, the assay solution required for spectrophotometric method was prepared as well as the irradiation steps. Each sample extraction was measured and calculated. The obtained results revealed that all samples were free from Diethylstilboesterol residues, the results were discussed.