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Rapid determination of organophosphorous pesticides in leeks by gas chromatography–triple quadrupole mass spectrometry
Authors:Lin-Juan Qu  Hui Zhang  Jian-Hua Zhu  Guo-Sheng Yang  Hassan Y Aboul-Enein
Affiliation:1. School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100, PR China;2. Shandong Supervision and Inspection Institute for Product Quality, Jinan 250100, PR China;3. Pharmaceutical and Medicinal Chemistry Department, National Research Centre, Dokki, Cairo 12311, Egypt;4. Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia (UTM), 81310 Skudai, Johor, Malaysia
Abstract:A rapid multi-residue method was developed for the determination of 20 organophosphorous pesticide residues in leeks by gas chromatography coupled to triple quadrupole mass spectrometry (GC–QqQ-MS/MS). The method was based on the modified QuEChERS sample preparation method. After microwave pre-treatment, leek samples were extracted with acetonitrile containing acetic acid 0.1% and cleaned by dispersive solid phase extraction. The QqQ analyser acquired data in selected reaction monitoring (SRM) mode. Recoveries of 20 organophosphorous pesticides ranged from 81.0% to 109.4% with the relative standard deviations (RSD) below 10.4%. The limits of detection (LODs) were 0.07–1.5 μg/kg. The limits of quantitation (LOQs) ranged from 0.25 to 5 μg/kg. Ten leek samples were analysed for method application.
Keywords:GC&ndash  QqQ-MS/MS  gas chromatography&ndash  triple quadrupole mass spectrometry  QqQ  triple quadrupole  QuEChERS  quick easy cheap effective rugged and safe  HAc  acetic acid  SRM  selected reaction monitoring  RSD  relative standard deviations  LOD  the limits of detection  LOQ  the limits of quantitation  GC&ndash  NPD  gas chromatography&ndash  nitrogen&ndash  phosphorus detector  GC&ndash  FPD  gas chromatography with flame photometric detector  GC&ndash  MS  gas chromatography&ndash  mass spectrometry  HPLC&ndash  MS  high performance liquid chromatography&ndash  mass spectrometry  GPC  gel permeation chromatography  SPE  solid phase extraction  PSA  primary secondary amine  GCB  graphitic carbon black  MgSO4  magnesium sulphate anhydrous  EI  electron impact ionisation  CID  collision-induced dissociation
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