Simultaneous determination of three pesticides and their metabolites in unprocessed foods using ultraperformance liquid chromatography-tandem mass spectrometry

ABSTRACT

We have developed a rapid, multi-compound analytical method for measuring residues of the pesticides thiamethoxam and its metabolite, clothianidin; fipronil and its three metabolites, fipronil sulfone, fipronil sulfide, and fipronil desulfinyl; and pyraclostrobin in unprocessed foods (rice, corn, cucumbers, tomatoes, apples, and bananas) by ultra-performance liquid chromatography coupled to tandem mass spectrometry. Acetonitrile was used as the extraction solvent, and an octadecylsilane-dispersive SPE was used to clean up the analytes, which were then separated through a UPLC HSS T3 column connected to a tandem mass spectrometer via an electrospray ionisation source. The linearity of this method for the target analytes was excellent (R² ≥0.990) in the concentration range of 5–1000 μg kg^–1. The average recoveries of the seven compounds at concentrations of 10, 100, and 1000 μg kg^–1 from six spiked matrix samples ranged from 73.6 to 110.6%, all with RSD values of ≤19.7%. The limit of quantification was 10 μg kg^–1. The method validated the effectiveness of the method for routine monitoring the residue of these pesticides and their metabolites in foods.

KEYWORDS:

• Pesticides
• metabolites
• residue
• QuEChERS
• UPLC-MS/MS
• unprocessed food

Acknowledgments

This study was supported by a grant from the National Natural Science Foundation of China (No. 31672057).

Disclosure statement

No potential conflict of interest was reported by the authors.

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Funding

This work was supported by the National Natural Science Foundation of China [31672057].