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High-throughput HPLC–MS/MS determination of the persistence of neonicotinoid insecticide residues of regulatory interest in dietary bee pollen

López-Fernández, Olalla, Rial-Otero, Raquel, Simal-Gándara, Jesus
Analytical and bioanalytical chemistry 2015 v.407 no.23 pp. 7101-7110
adsorbents, bee pollen, detection limit, hexane, high performance liquid chromatography, insecticide residues, neonicotinoid insecticides, silica, solid phase extraction, solvents, tandem mass spectrometry
The aim of this work is the development of a simple, fast, quantitative, and economic method for the determination of neonicotinoid insecticide residues in dietary bee pollen. Several parameters of the method, such as extraction solvent, extraction time, and solid-phase extraction sorbents for purification [silica, C₁₈, primary–secondary amine (PSA), and Envi-Carb II/PSA], were studied. The final proposed method based on solid–liquid extraction with hexane, cleanup with Supelclean™ Envi-Carb II/PSA cartridges, and subsequent analysis by high-performance liquid chromatography with tandem mass spectrometry was validated and applied to the analysis of commercial bee pollen samples from different geographical zones. Method performance was assessed by the evaluation of several quality parameters of the method, such as recovery values, repeatability, reproducibility, linearity, and limits of detection and quantification. Matrix effects on the chromatographic signal were also studied. The quality parameters of the method were equivalent to or better than those obtained with previously published methods, with recoveries between 81 and 99 % and repeatabilities lower than 8.8 %. The detection and quantification limits were in the ranges 0.2-2.2 μg kg⁻¹ and 0.4-4.3 μg kg⁻¹, respectively.