title: Determination of neonicotinoid insecticides and their metabolites in honey bee and honey by liquid chromatography tandem mass spectrometry.
abstract: The original analytical method for the simultaneous determination and confirmation of neonicotinoids insecticides (imidacloprid, clothianidin, acetamiprid, thiametoxam, thiacloprid, nitenpyram, dinotefuran) and some of their metabolites (imidacloprid guanidine, imidacloprid olefin, imidacloprid urea, desnitro-imidacloprid hydrochloride, thiacloprid-amid and acetamiprid-N-desmethyl) in honey bee and honey was developed. Preparation of honey bee samples involves the extraction with mixture of acetonitrile and ethyl acetate followed by cleaned up using the Sep-Pak Alumina N Plus Long cartridges. Honey samples were dissolved in 1% mixture of acetonitrile and ethyl acetate with addition of TEA, then extracts were cleaned up with Strata X-CW cartridges. The identity of analytes was confirmed using liquid chromatography tandem mass spectrometry. All compounds were separated on a Luna C18 column with gradient elution. The whole procedure was validated according to the requirements of SANCO 12571/2013. The average recoveries of the analytes ranged from 85.3% to 112.0%, repeatabilities were in the range of 2.8-11.2%, within-laboratory reproducibility was in the range of 3.3-14.6%, the limits of quantitation were in the range of 0.1-0.5μgkg(-1), depending of analyte and matrices. The validated method was successfully applied for the determination of clothianidin, imidacloprid and imidacloprid urea in real incurred honey bee samples and clothianidin in honey.
authors: Pharmacology and Toxicology Department, National Veterinary Research Institute (NVRI), al. Partyzantow 57, 24-100 Pulawy, Poland. Electronic address: malgorzata.gbylik@piwet.pulawy.pl.
authors: Malgorzata
authors: M
authors: Gbylik-Sikorska
authors: Pharmacology and Toxicology Department, National Veterinary Research Institute (NVRI), al. Partyzantow 57, 24-100 Pulawy, Poland.
authors: Tomasz
authors: T
authors: Sniegocki
authors: Pharmacology and Toxicology Department, National Veterinary Research Institute (NVRI), al. Partyzantow 57, 24-100 Pulawy, Poland.
authors: Andrzej
authors: A
authors: Posyniak
mesh_terms: D000818:Animals; D001516:Bees / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D006722:Honey / Q000032:analysis*; D007306:Insecticides / Q000032:analysis*; D057230:Limit of Detection; D016014:Linear Models; D010573:Pesticide Residues / Q000032:analysis*; D011725:Pyridines / Q000032:analysis*; D015203:Reproducibility of Results; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D007306:Insecticides; D010573:Pesticide Residues; D011725:Pyridines
keywords: Honey; Honey bee; LC-MS/MS; Metabolites; Neonicotinoids