Rapid determination of spirotetramat and its metabolite residues in milk by ultra performance liquid chromatography-tandem mass spectrometry

Abstract

A method for the rapid and simultaneous determination of spirotetramat (BYI08330) and its four metabolites in milk was developed with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted with acetonitrile for precipitating proteins, degreased with hexane, and analyzed by UPLC-MS/MS in positive electrospray ionization and multiple reaction monitoring (MRM) mode. Good linear relationships between peak areas and mass concentrations of the analytes were obtained in the range of 0.5-50 μ g/L with correlation coefficients greater than 0.998 (n=6). The limits of detection (LODs, S/N=3) and limits of quantification (LOQs, S/N=10) were 0.05-0.30 μ g/L and 0.17-1.00 μ g/L, respectively. The recoveries at the spiked levels of 1.0, 2.0 and 10 μ g/L were in the range of 80.0%-108.8% with relative standard deviations (RSDs) of 4.8%-15.2% (n=6). The method is fast, sensitive and accurate, and can be used to simultaneously determine BYI08330 and its four metabolites in milk.