Abstract: A method for the simultaneous determination of 7 sedatives in antler velvet of Cervus nippon Temminck by UPLC-MS/MS was developed by using pre-treatment technology of dispersive solid phase extraction. The antler velvet sample was treated with 2% aqueous ammonia ethyl acetate as an extractant and 200 mg C₁₈ as a purifying agent. Liquid chromatography conditions:ACQUITY BEH C₁₈ column(2.1 mm×100 mm,1.7 μm),mobile phase A was 0.1% formic acid acetonitrile,B was water,column temperature was 35 ℃. Mass spectrometry conditions:Positive ion mode(ESI⁺),multiple reactions monitoring mode. The sedative contents in antler velvet were quantified by external standard method. The linearity of the 7 sedatives in 0.3~100 ng/mL was good,the correlation coefficient R² was greater than 0.992,and the LOD of the 7 sedatives was 0.3 μg/kg,LOQ was 1 μg/kg,the average recovery rate was 82.6%~107.3%,and the RSD was less than 5%. The method had the advantages of simple operation,remarkable purification effect,high sensitivity,good accuracy and low detection limit. It could be used for the determination of 7 sedatives in antler velvet of Cervus nippon Temminck.