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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

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    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
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    † Canadian Food Inspection Agency, Calgary Laboratory, 3650-36th Street N.W., Calgary, Alberta T2L 2L1, Canada
    § ThermoFisher Scientific, 355 River Oaks Parkway, San Jose, California 95134, United States
    # Center for Food Safety and Applied Nutrition, U.S. Food and Drug Administration, 5100 Paint Branch Parkway, College Park, Maryland 20740, United States
    *(J. Wang) Phone: (403) 338-5273. Fax: (403) 338-5299. E-mail: [email protected]
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    Journal of Agricultural and Food Chemistry

    Cite this: J. Agric. Food Chem. 2014, 62, 42, 10375–10391
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    https://doi.org/10.1021/jf503778c
    Published September 29, 2014
    Copyright © 2014 American Chemical Society
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    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-MS2 (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-MS2 along with library matching showed great potential for identification and is being investigated further for routine practice.

    Copyright © 2014 American Chemical Society

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    Cite this: J. Agric. Food Chem. 2014, 62, 42, 10375–10391
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    https://doi.org/10.1021/jf503778c
    Published September 29, 2014
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