Abstract: | A rapid, reliable, and sensitive method is reported for the simultaneous analysis of pyrifluquinazon and its main metabolite NNI‐0101‐1H in fruits (strawberry and cherry) and vegetables (cucumber and tomato) using high‐performance liquid chromatography coupled with tandem mass spectrometry. A modified, quick, easy, cheap, effective, rugged, and safe procedure was used for the sample pre‐preparation. The target analytes were extracted with acetonitrile and then cleaned up using dispersive solid‐phase extraction procedure with primary secondary amine. Sample analysis was performed using electrospray ionization in positive mode. Good linearities with the correlation coefficients higher than 0.9991 were obtained in the range of 1–1000 μg/L under the optimized conditions. The average recoveries of the pyrifluquinazon and NNI‐0101‐1H were in the range of 71.4–106.0% with the relative standard deviations 1.8–11.8% in all matrices at three spiked levels (10, 100, and 1000 μg/kg). The limit of quantification 10 μg/kg was set as the lowest spiked level. The developed method is reliable and effective for the routine monitoring of pyrifluquinazon and its metabolite NNI‐0101‐1H in fruits and vegetables to ensure food safety. |