Simultaneous quantitative determination, identification and qualitative screening of pesticides in fruits and vegetables using LC-Q-Orbitrap™-MS

P. Zomer*, J.G.J. Mol

*Corresponding author for this work

    Research output: Contribution to journalArticleAcademicpeer-review

    73 Citations (Scopus)

    Abstract

    A method based on QuEChERS extraction and LC-quadrupole-Orbitrap™ MS detection was established utilising an
    improved fully non-targeted way of data acquisition with and without fragmentation. A full-scan acquisition event
    without fragmentation (resolving power 70 000) was followed by five consecutive fragmentation events (variable data
    independent acquisition – vDIA; resolving power 35 000) where all ions from the full-scan range are fragmented.
    Compared with fragmentation in a single event (all-ion fragmentation – AIF), this improves both selectivity and
    sensitivity for the fragment ions, which is beneficial for screening performance and identification capability. The
    method was validated, using the data from the same measurements, for two types of analysis: quantitation/identification
    and qualitative screening. The quantitative validation, performed according to the guidelines in SANCO/12571/
    2013, tested the performance of the method for 184 compounds in lettuce and orange at two spiking levels: 10 and
    50 ng g−1. The validation showed that the vast majority of the compounds met the criteria for trueness and precision
    set in the SANCO guidance document. In the qualitative validation the same 184 compounds were used to test the
    untargeted screening capabilities of the method. In this validation the compounds were spiked at three levels into 11
    different fruit and vegetable matrices, which were measured twice on separate days. Taking all data from the
    qualitative validation together, an overall detection rate of 92% was achieved at the 10 ng g−1 level, increasing to
    98% at 200 ng g−1. A screening detection limit (as defined in the SANCO guidelines) of 10 ng g−1 could be achieved
    for 134 compounds. For 39 and two pesticides the SDL was 50 and 200 ng g−1, respectively. For the other nine
    compounds no SDL could be established. The identification (ion ratio) criteria as recommended in the SANCO
    document could be met for 93% of the detected pesticide/matrix/concentration combinations. The outcome of both
    validations shows that the described method can be used to combine quantitative analysis and the identification of
    frequently detected pesticides (so far typically done using triple quadrupole MS/MS) with a qualitative screening to be
    used for a wide range of less frequent detected compounds in one measurement
    Original languageEnglish
    Pages (from-to)1628-1636
    JournalFood Additives & Contaminants. Pt. A, Chemistry, Analysis, Control, Exposure & Risk Assessment
    Volume32
    Issue number10
    DOIs
    Publication statusPublished - 2015

    Keywords

    • fruits
    • LC-MS
    • method validation
    • pesticides
    • vegetables

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