Rapid detection of fipronil and its metabolite residues in vegetables based on the UPLC-quadrupole-electrostatic field/orbital trap high resolution mass spectrometry / 国际药学研究杂志

ABSTRACT

Objective: To establish a method for the determination of fipronil and its metabolites in vegetables by ultra performance liquid chromatography-quadrupole-electrostatic field/orbital trap high resolution mass spectrometry. Methods: After homogenizing the vegetable samples, acetonitrile was added for ultrasonic extraction, then sodium chloride and anhydrous sodium sulfate were added to remove water. Finally, N- propyl ethylenediamine(PSA)powder, C18 powder and anhydrous sodium sulfate were added to remove impurities and purify the samples. Thermo Syncronis C18 column(100 mm×2.1 mm, 1.7 μm)was used for chromatographic separation of the samples. Data were collected under the Full MS-ddMS2 scanning mode of Q-Exactive high resolution mass spectrometry for qualitative and quantitative analysis. Results: The linearity of fipronil and its metabolites was good in the concentration range of 0.1-5.0 μg/L, and the correlation coefficient r2 were all greater than 0.9900. The average recovery of each component was 95.4%-108.6%, RSD was 0.769-5.563%, and RSD within 24 hours was 1.531%-4.959%. Conclusion: The present method appears to be simple, rapid, reproducible, stable and sensitive, which is suitable for rapid qualitative and quantitative detection of fipronil and its metabolites in vegetables.