Simulatneous determination of nitrapyrin and its metabolite residues in food crops by derivatization with gas chromatography-triple quadrupole mass spectrometry

A method based on precolumn derivatization along with gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) was developed for the determination of nitrapyrin and its metabolite, 6-chloropicolinic acid, in crops. The samples were extracted by acid acetonitrile, and subjected to precolumn derivatization using a sulfoacid. The quantification of the analytes was performed by the internal standard method. Good linear relationships between the peak areas and mass concentrations of the analytes were obtained in the range of 0.025-0.2 mg/L with correlation coefficients greater than 0.995 (n = 6). The limits of quantification (LOQs) were 0.05 mg/kg. The recoveries of the analytes in crops at three spiked levels (0.05, 0.1, and 0.2 mg/kg) were in the range of 80.4%-98.4%, with relative standard deviations between 1.0% and 10.1% (n = 6). This new method satisfies the related regulations for the determination of nitrapyrin and its metabolite in crops.