Pesticide contamination of bee products is a widespread phenomenon. Due to its composition, bee bread is affected by both lipophilic and hydrophilic substances. As proof of concept of a monitoring campaign and to better understand the extent of contamination, we developed an analytical method based on a modified QuEChERS extraction, with subsequent separation by liquid chromatography and detection by mass spectrometry. This allowed for the quantitation of 51 agricultural- or beekeeping-associated pesticides in bee bread. The workflow was applied to 60 samples taken biweekly throughout spring to autumn 2022 from five colonies at a Swiss apiary in an agricultural area. In total, 30 pesticides were identified (> LOD), among which 26 pesticides were quantitated. The total number of pesticides detected per colony ranged from 11 to 19. The most prevalent substances (> LOQ) were two neonicotinoid insecticides, acetamiprid and thiacloprid (max. 16 μg/kg and 37 μg/kg, respectively); seven fungicides, azoxystrobin (max. 72 μg/kg), boscalid (max. 50 μg/kg), cyprodinil (max. 1965 μg/kg), difenoconazole (max. 73 μg/kg), mandipropamid (max. 33 μg/kg), pyraclostrobin (max. 8 μg/kg) and trifloxystrobin (max. 38 μg/kg); and two herbicides, prosulfocarb (max. 38 μg/kg) and terbuthylazine (max. 26 μg/kg). The study revealed strong variability in pesticide occurrence and concentrations among colonies sampled at the same site and date. The applied biweekly sampling of bee bread from March to August was shown to be reliable in capturing peak contaminations and revealing the onset of certain pesticides in bee bread. The study provides an adequate practical approach for pesticide monitoring campaigns.
A method based on dynamic headspace vacuum transfer in trap extraction, followed by gas chromatography coupled with a mass spectrometer (DHS-VTT-GC-MS), was validated for the fast quantitation of 1,4-dichlorobenzene (p-dichlorobenzene; PDCB) and thymol residues in beeswax. The quantitation limits (LOQ) were 0.05 mg/kg (PDCB) and 0.25 mg/kg (thymol). Recoveries above 80% were obtained for PDCB concentrations between 0.05 and 10 mg/kg and for thymol concentrations between 0.25 and 200 mg/kg. Analysis of beeswax samples showed a good correlation between the results obtained by DHS-VTT-GC-MS analysis and those of a previous method based on SPE extraction followed by gas chromatography and triple- quadrupole mass spectrometry (GC-MS/MS) (R2 = 0.9770 for PDCB and 0.9666 for thymol). However, the sample preparation and chromatography were much shorter using the DHS-VTT-GC-MS method. Forty comb foundations samples produced in Switzerland in 2019 and 2021 were analysed using DHS-VTT-GC-MS. Fourteen samples contained PDCB above the LOQ of 0.05 mg/kg, ranging up to a maximum of 1.53 mg/kg. The mean concentration of the positive samples was 0.22 mg/kg. All samples contained thymol residues ranging between 3.9 and 84.4 mg/kg with mean and median concentrations of 22.7 mg/kg and 17.4 mg/kg. Residue levels of PCDB and thymol in Swiss beeswax were substantially below those measured 20 (PDCB) and 10 (thymol) years ago, respectively.
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