A method is developed for the determination of melengestrol acetate in bovine fat tissue at or less than the established tolerance level of 25 ppb. The procedure uses a combination of supercritical fluid extraction (SFE) and solid-phase extraction (SPE) techniques to produce an extract suitable for analysis with either high-performance liquid chromatography with ultraviolet detection or gas chromatography-mass spectrometry. Overall recovery of the analyte from bovine fat tissue is 99.4% with a coefficient of variation of 4.14%. The SFE-SPE procedure uses a total of 12 mL of organic solvent per fat tissue sample versus more than 1.7 L consumed in current extraction procedures.