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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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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author Omaira de la Hera
Aritza Izaguirre
Arrate Rivas
Rosa María Alonso
author_facet Omaira de la Hera
Aritza Izaguirre
Arrate Rivas
Rosa María Alonso
author_sort Omaira de la Hera
collection DOAJ
description 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.
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spelling doaj-art-8a30532b03d34e2d94e85c748246201f2024-11-26T18:21:58ZengMDPI AGSeparations2297-87392024-11-01111131710.3390/separations11110317QuEChERS-Based Method for the Determination of Fipronil in Protein Baits and <i>Vespa velutina</i> Larvae by HPLC-DAD and GC-MSOmaira de la Hera0Aritza Izaguirre1Arrate Rivas2Rosa María Alonso3FARMARTEM Group, Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Barrio Sarriena, s/n, 48940 Leioa, Biscay, SpainFARMARTEM Group, Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Barrio Sarriena, s/n, 48940 Leioa, Biscay, SpainFARMARTEM Group, Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Barrio Sarriena, s/n, 48940 Leioa, Biscay, SpainFARMARTEM Group, Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Barrio Sarriena, s/n, 48940 Leioa, Biscay, SpainProtein 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.https://www.mdpi.com/2297-8739/11/11/317QuEChERSchromatographyfipronilprotein bait <i>Vespa velutina larva</i>metabolism
spellingShingle Omaira de la Hera
Aritza Izaguirre
Arrate Rivas
Rosa María Alonso
QuEChERS-Based Method for the Determination of Fipronil in Protein Baits and <i>Vespa velutina</i> Larvae by HPLC-DAD and GC-MS
Separations
QuEChERS
chromatography
fipronil
protein bait <i>Vespa velutina larva</i>
metabolism
title QuEChERS-Based Method for the Determination of Fipronil in Protein Baits and <i>Vespa velutina</i> Larvae by HPLC-DAD and GC-MS
title_full QuEChERS-Based Method for the Determination of Fipronil in Protein Baits and <i>Vespa velutina</i> Larvae by HPLC-DAD and GC-MS
title_fullStr QuEChERS-Based Method for the Determination of Fipronil in Protein Baits and <i>Vespa velutina</i> Larvae by HPLC-DAD and GC-MS
title_full_unstemmed QuEChERS-Based Method for the Determination of Fipronil in Protein Baits and <i>Vespa velutina</i> Larvae by HPLC-DAD and GC-MS
title_short QuEChERS-Based Method for the Determination of Fipronil in Protein Baits and <i>Vespa velutina</i> Larvae by HPLC-DAD and GC-MS
title_sort quechers based method for the determination of fipronil in protein baits and i vespa velutina i larvae by hplc dad and gc ms
topic QuEChERS
chromatography
fipronil
protein bait <i>Vespa velutina larva</i>
metabolism
url https://www.mdpi.com/2297-8739/11/11/317
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AT arraterivas quechersbasedmethodforthedeterminationoffipronilinproteinbaitsandivespavelutinailarvaebyhplcdadandgcms
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