QuEChERS-Based Method for the Determination of Fipronil in Protein Baits and <i>Vespa velutina</i> Larvae by HPLC-DAD and GC-MS

Protein baits containing fipronil as a biocide have shown their effectivity as a control method for <i>Vespa velutina nigrithorax</i> (Lepeletier, 1836) in apiaries. This biocide is not selective for <i>Vespa velutina</i>, so it is important to use the minimum dose to inactiv...

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Bibliographic Details
Main Authors: Omaira de la Hera, Aritza Izaguirre, Arrate Rivas, Rosa María Alonso
Format: Article
Language:English
Published: MDPI AG 2024-11-01
Series:Separations
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Online Access:https://www.mdpi.com/2297-8739/11/11/317
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Summary:Protein baits containing fipronil as a biocide have shown their effectivity as a control method for <i>Vespa velutina nigrithorax</i> (Lepeletier, 1836) in apiaries. This biocide is not selective for <i>Vespa velutina</i>, so it is important to use the minimum dose to inactivate a nest. Therefore, the aim of this work was the development of analytical methods for the determination of fipronil in protein baits for quality control purposes and in larvae of <i>Vespa velutina</i> to determine the biocide content after protein bait ingestion and to acquire knowledge on fipronil metabolism in larvae. For this purpose, a Quechers-based HPLC-PDA method was developed and validated for the determination of fipronil in both matrixes. Furthermore, a GC-MS method was developed for the analysis of fipronil and its metabolites in dead <i>Vespa velutina</i> larvae fed with a mash containing 0.01% fipronil. Quechers-based HPLC-DAD allowed for the determination of the fipronil content in baits. Fipronil and the metabolites fipronil sulfone and fipronil sulfide were identified by GC-MS in extracts of larvae fed with a protein mash containing 0.01% fipronil. The transformation of fipronil into fipronil sulfone inside the larvae and the high toxicity of this metabolite open the possibility to produce protein baits with lower biocide concentrations.
ISSN:2297-8739