Abstract: A method for determination of zeranol and related compounds（talernol, zearalanone, -zearalenol）in bovine muscle by gas chromatography-mass spectrometry was described. The samples were extracted with methanol, condensed, diluted with water and extracted with ethyl acetate. Then hexane was added to remove the fat, The solution was extracted with KOH and then with a ether, cleaned up with NH2-SPE, After derivatization, the samples were analysed by gas chromatography-mass spectrometry. The linear range was 0.5-10.0ng/g and the limit of detection was 1.0 ng/g. Recoveries were 71.5%-81.4% with CVs of 1.4%-5.0% at spiked levels of 5.0 ng/g.