In the period from August 1981 to April 1983, 10243 random samples of urine from slaughtered cattle were inspected for the presence of the stilbene derivatives diethylstilbestrol (DES), dienestrol (DE), and hexestrol (HEX). Fast screening of all samples was performed by radioimmunoassay (RIA) with prior clean‐up column chromatography. In this screening, 216 samples were indicated for confirmatory analyses by combined high performance liquid chromatography‐gas chromatography‐mass spectrometry (HPLC‐GCMS) on account of an immunochemical response equivalent to 1 μg/ 1 DES or more. The presence of DES was confirmed in 184 samples, DE in 5 samples and HEX in 14 samples. In the remaining 13 samples no stilbene derivative could be confirmed.