title: Ultrahigh-performance liquid chromatography electrospray ionization Q-Orbitrap mass spectrometry for the analysis of 451 pesticide residues in fruits and vegetables: method development and validation.
abstract: This paper presents an application of ultrahigh-performance liquid chromatography electrospray ionization quadrupole Orbitrap high-resolution mass spectrometry (UHPLC/ESI Q-Orbitrap MS) for the determination of 451 pesticide residues in fruits and vegetables. Pesticides were extracted from samples using the QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure. UHPLC/ESI Q-Orbitrap MS in full MS scan mode acquired full MS data for quantification, and UHPLC/ESI Q-Orbitrap Full MS/dd-MS(2) (i.e., data-dependent scan mode) obtained product ion spectra for identification. UHPLC/ESI Q-Orbitrap MS quantification was achieved using matrix-matched standard calibration curves along with the use of isotopically labeled standards or a chemical analogue as internal standards to achieve optimal method accuracy. The method performance characteristics include overall recovery, intermediate precision, and measurement uncertainty evaluated according to a nested experimental design. For the 10 matrices studied, 94.5% of the pesticides in fruits and 90.7% in vegetables had recoveries between 81 and 110%; 99.3% of the pesticides in fruits and 99.1% of the pesticides in vegetables had an intermediate precision of ≤20%; and 97.8% of the pesticides in fruits and 96.4% of the pesticides in vegetables showed measurement uncertainty of ≤50%. Overall, the UHPLC/ESI Q-Orbitrap MS demonstrated acceptable performance for the quantification of pesticide residues in fruits and vegetables. The UHPLC/ESI Q-Orbitrap Full MS/dd-MS(2) along with library matching showed great potential for identification and is being investigated further for routine practice.
authors.affiliation: Canadian Food Inspection Agency, Calgary Laboratory, 3650-36th Street N.W., Calgary, Alberta T2L 2L1, Canada.
authors.forename: Jian
authors.initials: J
authors.lastname: Wang
authors.forename: Willis
authors.initials: W
authors.lastname: Chow
authors.forename: James
authors.initials: J
authors.lastname: Chang
authors.forename: Jon W
authors.initials: JW
authors.lastname: Wong
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005506:Food Contamination / Q000032:analysis; D005638:Fruit / Q000737:chemistry*; D013058:Mass Spectrometry / Q000379:methods*; D010573:Pesticide Residues / Q000737:chemistry*; D014675:Vegetables / Q000737:chemistry*
chemical_list: D010573:Pesticide Residues
keywords: UHPLC/ESI Q-Orbitrap; fruits and vegetables; high-resolution mass spectrometer; identification; measurement uncertainty; pesticides; quantification