Development and validation of an ultra performance liquid chromatography Q-Exactive Orbitrap mass spectrometry for the determination of fipronil and its metabolites in tea and chrysanthemum

A fast, sensitive and reliable method for the determination of fipronil and its metabolites in tea and chrysanthemum was developed using a modified QuEChERS technique and an ultra performance liquid chromatography Q-Exactive Orbitrap mass spectrometry. The mixture of adsorbents containing primary secondary amine (PSA), octadecylsilane (C18) and carbon nanotubes (CNTs), was used as QuEChERS adsorbents. The use of mass resolution at 70000 full width at half maximum (FWHM) and narrow mass windows at 5 ppm achieved high selectivity and repeatability. Satisfactory linearity with correlative coefficient (R2) higher than 0.996 was achieved for all compounds. Recoveries at three levels (2, 10 and 50 μg kg−1) ranged from 86% to 112%, while the intra- and inter-day accuracies were less than 15%. Limits of quantification for fipronil and its metabolites were 2 μg kg−1, which fulfils the requirement of maximum residue limits formulated by European Union and Japan.