Abstract
A novel, rapid and simple magnetic solid-phase extraction (MSPE) method combined with ultra-high performance liquid chromatography coupled with Q-Exactive high resolution mass spectrometry (UHPLC-Q-Exactive HRMS) was proposed for determination of fipronil and its metabolites in egg samples. In this study, novel polydopamine functionalized magnetic core-shell mesoporous silica nanoparticles (Fe3O4@nSiO2@mSiO2-PDA) were used as MSPE adsorbent for purification and enrichment of fipronil and its metabolites for the first time. The proposed method showed a good linearity (R2 ≥ 0.997), high sensitivity (limit of detection in the range of 0.002–0.004 μg/kg and limit of quantification in the range of 0.006–0.010 μg/kg), adequate recovery (80.6–95.3%) and repeatability (intra-day precision in the range of 2.2–6.7% and inter-day precision in the range of 4.4–10.7%). Finally, the developed MSPE-UHPLC-Q-Exactive HRMS method was successfully applied for determination of fipronil and its metabolites in egg samples.
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