title: Multiresidue pesticide analysis in fresh produce by capillary gas chromatography-mass spectrometry/selective ion monitoring (GC-MS/SIM) and -tandem mass spectrometry (GC-MS/MS).
abstract: A multiresidue method for the analysis of pesticides in fresh produce has been developed using salt-out acetonitrile extraction, solid-phase dispersive cleanup with octadecyl-bonded silica (C(18)), and graphitized carbon black/primary-secondary amine (GCB/PSA) sorbents and toluene, followed by capillary gas chromatography-mass spectrometry in selected ion monitoring mode (GC-MS/SIM) or -tandem mass spectrometry (GC-MS/MS). Quantitation was determined from calibration curves using matrix-matched standards ranging from 3.3 to 6667 ng/mL with r(2) > 0.99, and geometric mean limits of quantitation were typically 8.4 and 3.4 microg/kg for GC-MS/SIM and GC-MS/MS, respectively. Identification was determined by using target and qualifier ions and qualifier-to-target ratios for GC-MS/SIM and two ion transitions for GC-MS/MS. Fortification studies (10, 25, 100, and 500 microg/kg) were performed on 167 organohalogen, organophosphorus, and pyrethroid pesticides in 10 different commodities (apple, broccoli, carrot, onion, orange, pea, peach, potato, spinach, and tomato). The mean percent recoveries were 90 +/- 14, 87 +/- 14, 89 +/- 14, and 92 +/- 14% for GC-MS/SIM and 95 +/- 22, 93 +/- 14, 93 +/- 13, and 97 +/- 13% for GC-MS/MS at 10, 25, 100, and 500 microg/kg, respectively. GC-MS/MS was shown to be more effective than GC-MS/SIM due to its specificity and sensitivity in detecting pesticides in fresh produce samples. The method, based on concepts from the multiresidue procedure used by the Canadian Food Inspection Agency and QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe), was shown to be efficient in screening, identifying, and quantitating pesticides in fresh produce samples.
authors.affiliation: Center for Food Safety and Applied Nutrition, Office of Regulatory Science, US Food and Drug Administration, HFS-706, 5100 Paint Branch Parkway, College Park, Maryland 20740-5350, USA. jon.wong@fda.hhs.gov
authors.forename: Jon W
authors.initials: JW
authors.lastname: Wong
authors.forename: Kai
authors.initials: K
authors.lastname: Zhang
authors.forename: Katherine
authors.initials: K
authors.lastname: Tech
authors.forename: Douglas G
authors.initials: DG
authors.lastname: Hayward
authors.forename: Carolyn M
authors.initials: CM
authors.lastname: Makovi
authors.forename: Alexander J
authors.initials: AJ
authors.lastname: Krynitsky
authors.forename: Frank J
authors.initials: FJ
authors.lastname: Schenck
authors.forename: Kaushik
authors.initials: K
authors.lastname: Banerjee
authors.forename: Soma
authors.initials: S
authors.lastname: Dasgupta
authors.forename: Don
authors.initials: D
authors.lastname: Brown
mesh_terms: D002138:Calibration; D005506:Food Contamination / Q000032:analysis; D005638:Fruit / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D007306:Insecticides / Q000032:analysis; D009943:Organophosphorus Compounds / Q000032:analysis; D010573:Pesticide Residues / Q000032:analysis*; D011722:Pyrethrins / Q000032:analysis; D011786:Quality Control; D012680:Sensitivity and Specificity; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014675:Vegetables / Q000737:chemistry*
chemical_list: D007306:Insecticides; D009943:Organophosphorus Compounds; D010573:Pesticide Residues; D011722:Pyrethrins