A field study was performed to assess the drug residue level in edible tissues after a therapeutic application of the synthetic glucocorticoids dexamethasone and flumethasone. Three diseased calves were injected intramuscularly with a commercial batch of dexamethasone esters and slaughtered 72 h after treatment. Another three calves were injected intramuscularly with an aqueous flumethasone preparation and slaughtered 24 h later. Residues of synthetic glucocorticoids in liver, muscle, kidney, and urine were assessed by competitive enzyme immunoassay. All dexamethasone concentrations exceeded the maximal residue level of 0.75 microg/kg in muscle and kidney and 2 microg/kg in the liver. The presence of both dexamethasone and flumethasone in the liver was confirmed by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). These results indicate that liver tissue provides a suitable matrix to monitor the presence of illegal residues of synthetic glucocorticoids in slaughtered animals.