Molecularly imprinted polymer materials were prepared by bulk polymerization and precipitation polymerization methods using diazepam as template molecular，and effects of cross-linker，porogen agent and temperature on the properties of polymer materials were optimized.The molecularly imprinted micropheres were sythesized with divinylbenzene(DVB) as cross-linker and acetonitrile as porogen agent.The polymer prepared by bulk polymerization showed irregular shape，while the micropheres prepared by precipitation polymerization were regular in SEM image.The binding capacity and selective characteristics of the molecularly imprinted polymer were investigated by equilibrium binding experiments.It showed that the maximum adsorption to diazepam of the molecularly imprinted micropheres is up to 130 μg/g and the adsorption to oxazepam and nitrazepam is about 110 μg/g.The results showed that the imprinted polymer exhibited higher adsorptivity and selectivity for diazepam compared with the non-imprinted polymers.In addition，the molecularly imprinted polymer was used as solid phase extraction sorbent in solid phase extraction column to isolate diazepam in feed and pig urine samples for its excellent identifying characteristics.High performance liquid chromatography(HPLC) was imployed to detect three drugs.The method showed good linearities in the range of 0.1-20 mg/L for oxazepam,nitrazepam and diazepam，with correlation coefficients of 0.999 6-0.999 9 and detection limits(S/N=3 ) of 0.03-0.08 mg/L.The recoveries of three drug in feed and pig urine were in the range of 71%-79% and 66%-71%，respectively.The proposed method provides a new way for the detection of antipsychotic drugs.