title: Determination of traces of fipronil and its metabolites in pollen by liquid chromatography with electrospray ionization-tandem mass spectrometry.
abstract: Fipronil is a pesticide suspected of having harmful effects on honey bees at microgram per kilogram levels. Considering the lack of methodology, it thus appeared to be necessary to develop a method for the determination of the lowest amounts of fipronil and its metabolites in pollen. This paper describes a new analytical method with a limit of quantification (LOQ) of 0.1 microg/kg for a representative sample weight of 5 g. In the case of a field study, this tool was used for checking the possible existence of fipronil and/or metabolites in pollen samples, but none of them contained residues higher than the LOQ. This three-step rapid method uses liquid-solid solvent extraction with mechanical grinding, followed by liquid-liquid partitioning and Florisil solid-phase extraction for the two cleanup steps. The quantification is made by liquid chromatography with electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS). Indeed, combined with an adequate sample treatment, this technique offers good sensitivity and selectivity in such a complex matrix. The method has given good recoveries of 74-104% with relative standard deviations of 5.6-18.2%.
authors.affiliation: Agence Française de Sécurité Sanitaire des Aliments (AFSSA), Laboratoire d'Etudes et de Recherches sur les Petits Ruminants et les Abeilles, 105 route des Chappes, F-06902 Sophia Antipolis Cedex, France. a.kadar@afssa.fr
authors.forename: Ali
authors.initials: A
authors.lastname: Kadar
authors.forename: Jean-Paul
authors.initials: JP
authors.lastname: Faucon
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D007306:Insecticides / Q000032:analysis* / Q000378:metabolism; D011058:Pollen / Q000737:chemistry*; D011720:Pyrazoles / Q000032:analysis* / Q000378:metabolism*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
chemical_list: D007306:Insecticides; D011720:Pyrazoles; C082360:fipronil