PMID- 26654830 OWN - NLM STAT- MEDLINE DCOM- 20160725 LR - 20181202 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1426 DP - 2015 Dec 24 TI - A sensitive and efficient method for routine pesticide multiresidue analysis in bee pollen samples using gas and liquid chromatography coupled to tandem mass spectrometry. PG - 161-73 LID - S0021-9673(15)01743-4 [pii] LID - 10.1016/j.chroma.2015.11.081 [doi] AB - Several clean-up methods were evaluated for 253 pesticides in pollen samples concentrating on efficient clean-up and the highest number of pesticides satisfying the recovery and precision criteria. These were: (a) modified QuEChERS using dSPE with PSA+C18; (b) freeze-out prior to QuEChERS using dSPE with PSA+C18; (c) freeze-out prior to QuEChERS using dSPE with PSA+C18+Z-Sep; and (d) freeze-out followed by QuEChERS using dSPE with PSA+C18 and SPE with Z-Sep. Determinations were made using LC-MS/MS and GC-MS/MS. The modified QuEChERS protocol applying a freeze-out followed by dSPE with PSA+C18 and SPE clean-up with Z-Sep was selected because it provided the highest number of pesticides with mean recoveries in the 70-120% range, as well as relative standard deviations (RSDs) typically below 20% (12.2% on average) and ensured much better removal of co-extracted matrix compounds of paramount importance in routine analysis. Limits of quantification at levels as low as 5mugkg(-1) were obtained for the majority of the pesticides. The proposed methodology was applied to the analysis of 41 pollen bee samples from different areas in Spain. Pesticides considered potentially toxic to bees (DL50<2mug/bee) were detected in some samples with concentrations up to 72.7mugkg(-1), which could negatively affect honeybee health. CI - Copyright (c) 2015 Elsevier B.V. All rights reserved. FAU - Vazquez, P Parrilla AU - Vazquez PP AD - Agrifood Campus of International Excellence (ceiA3), European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, Department of Chemistry and Physics, University of Almeria, La Canada de San Urbano, 04120 Almeria, Spain. FAU - Lozano, A AU - Lozano A AD - Agrifood Campus of International Excellence (ceiA3), European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, Department of Chemistry and Physics, University of Almeria, La Canada de San Urbano, 04120 Almeria, Spain. FAU - Ucles, S AU - Ucles S AD - Agrifood Campus of International Excellence (ceiA3), European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, Department of Chemistry and Physics, University of Almeria, La Canada de San Urbano, 04120 Almeria, Spain. FAU - Ramos, M M Gomez AU - Ramos MM AD - Agrifood Campus of International Excellence (ceiA3), European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, Department of Chemistry and Physics, University of Almeria, La Canada de San Urbano, 04120 Almeria, Spain. FAU - Fernandez-Alba, A R AU - Fernandez-Alba AR AD - Agrifood Campus of International Excellence (ceiA3), European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, Department of Chemistry and Physics, University of Almeria, La Canada de San Urbano, 04120 Almeria, Spain. Electronic address: amadeo@ual.es. LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20151128 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Pesticide Residues) SB - IM MH - Animals MH - *Bees MH - Chromatography, Liquid/methods MH - Pesticide Residues/*analysis MH - Pollen/*chemistry MH - Solid Phase Extraction MH - Spain MH - Tandem Mass Spectrometry/methods OTO - NOTNLM OT - Freezing-out OT - GC-MS/MS OT - LC-MS/MS OT - Multiresidue pesticide analysis OT - Pollen OT - Zirconium dioxide EDAT- 2015/12/15 06:00 MHDA- 2016/07/28 06:00 CRDT- 2015/12/15 06:00 PHST- 2015/08/03 00:00 [received] PHST- 2015/11/24 00:00 [revised] PHST- 2015/11/25 00:00 [accepted] PHST- 2015/12/15 06:00 [entrez] PHST- 2015/12/15 06:00 [pubmed] PHST- 2016/07/28 06:00 [medline] AID - S0021-9673(15)01743-4 [pii] AID - 10.1016/j.chroma.2015.11.081 [doi] PST - ppublish SO - J Chromatogr A. 2015 Dec 24;1426:161-73. doi: 10.1016/j.chroma.2015.11.081. Epub 2015 Nov 28.