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Trace Analysis of Seven Neonicotinoid Insecticides in Bee Pollen by Solid–Liquid Extraction and Liquid Chromatography Coupled to Electrospray Ionization Mass Spectrometry

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Abstract

A new, fast, simple, and efficient sample treatment to extract seven neonicotinoid insecticides (acetamiprid, clothianidin, dinotefuran, imidacloprid, nitenpyram, thiacloprid, and thiamethoxam) in corbicular bee pollen has been developed. This procedure consisted of a solid–liquid extraction of the neonicotinoids from pollen with dichloromethane, followed by evaporation and reconstitution. Once the neonicotinoids were extracted, they were determined using a liquid chromatography coupled to an electrospray ionization mass spectrometry method. The method was validated in terms of selectivity, linearity, precision and recovery. The limits of detection and quantification were 0.4–2.8 μg/kg and 1.2–9.1 μg/kg, respectively, and the extraction recoveries were between 86 and 106 % in all cases. Finally, the proposed method was applied to analyze bee pollen samples collected from apiaries located close to fruit orchards in two Spanish regions, and traces of acetamiprid and imidacloprid were found in two samples.

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Abbreviations

QC:

Quality control

SIM:

Selected ion monitoring

FIA:

Flow injection analysis

CAR:

Centro Apícola Regional

ESI:

Electrospray ionization

MRLs:

Maximum residue levels

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Acknowledgments

Authors wish to thank Prof. Dr. Pilar de la Rua and the CAR of Marchamalo for supplying the bee pollen samples. M.T. Martín would like to thank the Spanish Ministry for her “Ramon y Cajal” contract, and K. P. Yáñez wish also to thank the E.U. ERASMUS-MUNDUS program for her PhD grant. This work was funded by the Spanish MARM-FEAGA (Programa Nacional Apícola 2011–2013).

Conflict of Interest

Karen P. Yáñez declares that she has no conflict of interest. José L. Bernal declares that he has no conflict of interest. María J. Nozal declares that she has no conflict of interest. María T. Martín declares that she has no conflict of interest. José Bernal declares that he has no conflict of interest. This article does not contain any studies with human or animal subjects.

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Correspondence to José Bernal.

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Yáñez, K.P., Martín, M.T., Bernal, J.L. et al. Trace Analysis of Seven Neonicotinoid Insecticides in Bee Pollen by Solid–Liquid Extraction and Liquid Chromatography Coupled to Electrospray Ionization Mass Spectrometry. Food Anal. Methods 7, 490–499 (2014). https://doi.org/10.1007/s12161-013-9710-9

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  • DOI: https://doi.org/10.1007/s12161-013-9710-9

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