A fatal intoxication due to the ingestion of tilidine, a narcotic analgesic, in conjunction with ethanol, is described. Tilidine and its two active metabolites, nortilidine and bisnortilidine, were identified and quantitated in the biological fluids and tissues by thin-layer chromatography (TLC), gas-liquid chromatography with sensitive nitrogen-phosphorus detection (GLC/NPD) and gas-liquid chromatography with mass spectrometric detection (GC/MS). The toxicological results are compared with previously reported 14C-tilidine tissue distributions in rats following oral administration and limited tissue data in a previously reported human fatality. In the present case, the death was attributed to the combined central nervous system-depressing effects of ethanol and tilidine.