PMID- 27447929 OWN - NLM STAT- MEDLINE DCOM- 20170209 LR - 20191210 IS - 1873-376X (Electronic) IS - 1570-0232 (Linking) VI - 1031 DP - 2016 Sep 15 TI - Simultaneous determination of eight neonicotinoid insecticide residues and two primary metabolites in cucumbers and soil by liquid chromatography-tandem mass spectrometry coupled with QuEChERS. PG - 15-28 LID - S1570-0232(16)30396-8 [pii] LID - 10.1016/j.jchromb.2016.06.020 [doi] AB - A new, rapid, sensitive, precise and validated high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) method was developed for the simultaneous determination of eight neonicotinoid insecticides with their two primary metabolites in cucumbers and soil based on QuEChERS as a pretreatment procedure. In QuEChERS procedure, cucumber samples were extracted with acetonitrile and cleaned using (C18 sorbent material), while soil samples were extracted with a mixture of acetonitrile:dichloromethane (8.3:16.7v:v). The LC-MS/MS conditions were optimized to provide good selectivity and specificity of the developed method where neonicotinoids were separated using gradient elution of water and acetonitrile both containing 0.1% formic acid with Gemini C18 column where the last compound was eluted at 9.5min. Average recoveries of the eight neonicotinoids and their metabolites ranged between 81.6% and 95.7% in fortified cucumber samples with relative standard deviations (RSDs) lower than 13.18% and between 80.3% and 104% in fortified soil samples with relative standard deviations (RSDs) lower than 8.44%. The limits of detection (LODs) and quantification (LOQs) for the ten compounds were in the ranges of (0.08-6.06ng/g) and (0.26-20ng/g), respectively. The method was applied successfully to determine residues and rate of disappearance of the eight neonicotinoids from cucumber and soil and their half-lives where a safety pre-harvest interval of 5days for acetampirid, 12days for imidacloprid, 15days for nitenpyram, 12days for thiamethoxam, 5days for flonicamid, 8days for clothianidin, 2days for Dinotefuran, and 1day for thiacloprid were suggested. CI - Copyright (c) 2016 Elsevier B.V. All rights reserved. FAU - Abdel-Ghany, Maha F AU - Abdel-Ghany MF AD - Pharmaceutical Analytical Chemistry Department, Faculty of pharmacy, Ain Shams University, Cairo, Egypt. FAU - Hussein, Lobna A AU - Hussein LA AD - Pharmaceutical Analytical Chemistry Department, Faculty of pharmacy, Ain Shams University, Cairo, Egypt. FAU - El Azab, Noha F AU - El Azab NF AD - Pharmaceutical Analytical Chemistry Department, Faculty of pharmacy, Ain Shams University, Cairo, Egypt. Electronic address: noha_3zab@yahoo.com. FAU - El-Khatib, Ahmed H AU - El-Khatib AH AD - Pharmaceutical Analytical Chemistry Department, Faculty of pharmacy, Ain Shams University, Cairo, Egypt; Department of Chemistry, Humboldt-Universitat zu Berlin, Berlin, Germany. FAU - Linscheid, Michael W AU - Linscheid MW AD - Department of Chemistry, Humboldt-Universitat zu Berlin, Berlin, Germany. LA - eng PT - Journal Article PT - Validation Study DEP - 20160616 PL - Netherlands TA - J Chromatogr B Analyt Technol Biomed Life Sci JT - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JID - 101139554 RN - 0 (Insecticides) RN - LMS11II2LO (Anabasine) SB - IM MH - Anabasine/*analysis/metabolism MH - Chromatography, High Pressure Liquid/*methods MH - Cucumis sativus/*metabolism MH - Insecticides/*analysis/metabolism MH - Limit of Detection MH - Reproducibility of Results MH - Tandem Mass Spectrometry/*methods OTO - NOTNLM OT - Cucumber OT - MS/MS OT - Metabolites OT - Neonicotinoids OT - QuEChERS OT - Soil EDAT- 2016/07/23 06:00 MHDA- 2017/02/10 06:00 CRDT- 2016/07/23 06:00 PHST- 2016/02/24 00:00 [received] PHST- 2016/06/08 00:00 [revised] PHST- 2016/06/13 00:00 [accepted] PHST- 2016/07/23 06:00 [entrez] PHST- 2016/07/23 06:00 [pubmed] PHST- 2017/02/10 06:00 [medline] AID - S1570-0232(16)30396-8 [pii] AID - 10.1016/j.jchromb.2016.06.020 [doi] PST - ppublish SO - J Chromatogr B Analyt Technol Biomed Life Sci. 2016 Sep 15;1031:15-28. doi: 10.1016/j.jchromb.2016.06.020. Epub 2016 Jun 16.