title: Collaborative validation of the QuEChERS procedure for the determination of pesticides in food by LC-MS/MS.
abstract: Seven FDA pesticide laboratories collaborated to develop and validate an LC-MS/MS method to determine 173 pesticides in <20 min. The average determination coefficient (r²) was >0.99 for all but two compounds tested. The limits of detection were <20 ng/mL for all compounds and <10 ng/mL for 363 of the 368 transitions reported. The method was used to determine pesticides in two AOAC sponsored proficiency samples. The LC-MS/MS determination was used for the analysis of oranges, carrots and spinach using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) method. Each matrix was fortified at 20, 100, 400, and 1000 ng/g. No false positive responses were detected in controls of the three matrices. 165 pesticides had recoveries between 70 and 130%, and 161 had minimum detection levels less than 10 ng/g. Recoveries of 169 compounds for the 1000 ng/g spikes were within 50-150%. A matrix effect study indicated all three matrices caused a small net suppressing effect, the most pronounced attributable to the citrus matrix. The procedure proved to be accurate, precise, linear, sensitive and rugged, and adds 100 pesticides to the scope of the FDA pesticide program.
authors.affiliation: Total Diet and Pesticide Research Center, Kansas District Lab, KAN, U.S. Food and Drug Administration , 11510 W 80th Street, Lenexa, Kansas 66214, USA.
authors.forename: Chris
authors.initials: C
authors.lastname: Sack
authors.forename: Michael
authors.initials: M
authors.lastname: Smoker
authors.forename: Narong
authors.initials: N
authors.lastname: Chamkasem
authors.forename: Richard
authors.initials: R
authors.lastname: Thompson
authors.forename: Greg
authors.initials: G
authors.lastname: Satterfield
authors.forename: Claude
authors.initials: C
authors.lastname: Masse
authors.forename: Greg
authors.initials: G
authors.lastname: Mercer
authors.forename: Barbara
authors.initials: B
authors.lastname: Neuhaus
authors.forename: Irene
authors.initials: I
authors.lastname: Cassias
authors.forename: Eugene
authors.initials: E
authors.lastname: Chang
authors.forename: Yi
authors.initials: Y
authors.lastname: Lin
authors.forename: Shaun
authors.initials: S
authors.lastname: Macmahon
authors.forename: Jon
authors.initials: J
authors.lastname: Wong
authors.forename: Kai
authors.initials: K
authors.lastname: Zhang
authors.forename: Robert E
authors.initials: RE
authors.lastname: Smith
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D005506:Food Contamination / Q000032:analysis*; D005638:Fruit / Q000737:chemistry*; D010573:Pesticide Residues / Q000032:analysis* / Q000302:isolation & purification; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014675:Vegetables / Q000737:chemistry*
chemical_list: D010573:Pesticide Residues