Purified by solid phase extraction column, using C₁₈ column as separation column and formic water-acetonitrile as flow phase for gradient elution, qualitative and quantitative analysis of characteristic ions of target compounds were detected by LC-MS/MS in MRM mode. Results, this method was in the linear range of 0.1～10.0 μg/mL, linear correlation coefficient of ＞0.999 0, the detection limit of the method was 0.01 mg/kg, and the quantitative limit was 0.03 mg/kg. At the spiking levels of 0.03, 0.10, and 0.50 mg/kg, the recovery rate of the method was 88.3%～95.0%, with RSD was 5.2%～8.8%. The method has the advantages of simple pretreatment, low amount of organic solvent, short analysis time, good selectivity and high sensitivity. The method is suitable for the detection of anilazine in tomatoes and cucumbers.