Objective To establish a method for the detection of 3-nitropropionic acid in sugarcane by solid-phase extraction(SPE) coupled with ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods Samples were extracted by acetonitrile and cleaned up by Sep-pak NH2 solid phase extraction column.The 3-nitropropionic acid was determined by UPLC-MS/MS.The chromatographic conditions: using Waters ACQUITY BEH C18 column(1.7 μm,50 mm×2.1 mm) with water as mobile phase A and acetonitrile as mobile phase B for gradient elution;keeping the column temperature at 40 ℃ and the samples at 10 ℃ with an injection volume of 5 μl.Results There was a good linearity of the calibration curve for 3-nitropropionic acid standard in the range of 4.0-40.0 μg/kg with correlation coefficient of 0.998.The detection limit of the method was 1.0 μg/kg and the limit of quantification was 4.0 μg/kg.The average recovery at three spiked levels was in the range of 92.5%-93.6%,and the relative standard derivation was lower than 10%.Conclusion The method is simple,rapid,sensitive and accurate,which can be used in the detection of 3-nitropropionic acid in sugar cane.