Abstract: A new solid phase extraction-liquid chromatography-tandem mass spectrometry（SPE-LC-MS/MS）method for simultaneous determination of 1,2-stilbenes, diethylstilbestrol (DES), dienoestrol (DIS) and hexestrol (HES) in animal tissues was reported. The 1,2-stilbenes were extracted with methanol from analyte by ultrasonic. The extraction was evaporated (40 ℃) to 5 mL, purified by passing through HLB（20 g•L^-1）solidphase extraction cartridges. The elution was evaporated by nitrogen blow and dissolved by mobile phase, and then assayed by liquid chromatography-electrospray ionization tandem mass spectrometry. The limits of detection(LOD) are 0.2 μg•kg^-1, and the limits of quantitation(LOQ) are 0.5 μg•kg^-1. The calibration curves are linear between 1.0 μg•L^-1 and 100 μg•L^-1 for 1,2-stilbenes. Recoveries of DES, DIS, HES in animal tissues are 78.8％～110.9％, and inter-relative standard deviation（n=5）are less than 8.0%, respectively, at spiked levels of 0.5～20 μg•kg^-1. The method is simple, sensitive and reliable for food safety.