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Analytical and Bioanalytical Chemistry

, Volume 411, Issue 7, pp 1421–1431 | Cite as

Non-target data acquisition for target analysis (nDATA) of 845 pesticide residues in fruits and vegetables using UHPLC/ESI Q-Orbitrap

  • Jian WangEmail author
  • Willis Chow
  • Jon W. Wong
  • Daniel Leung
  • James Chang
  • Mengmeng Li
Research Paper

Abstract

A non-target data acquisition for target analysis (nDATA) workflow based on accurate mass measurements using UHPLC/ESI Q-Orbitrap full MS-data-independent acquisition and a compound database was developed to screen pesticide residues in fruit and vegetable samples. The compound database of 845 pesticides was built from dd-MS2 (data-dependent acquisition) product ion spectral data and LC retention times of individual pesticide standards. MS2 spectra of samples were acquired using multiplexing data-independent acquisition (mDIA) and variable data-independent acquisition (vDIA). Screening of pesticides in samples was based on either the retention time (± 0.5 min) and the mass accuracy (± 5 ppm) of a precursor (RTP by full MS) or the retention time (± 0.5 min) and the mass accuracy (± 5 ppm) of a precursor and its fragment ion (RTFI by full MS/DIA). In validation studies involving mDIA and vDIA analysis of 10 fruits and vegetables spiked with pesticides prior to QuEChERS sample preparation, RTP correctly found up to 765 and 796 pesticides at 10 and 100 μg/kg, respectively, whereas RTFI correctly identified up to 729 and 764 pesticides at the same respective concentrations. UHPLC/ESI Q-Orbitrap full MS/mDIA or vDIA proved to be a comprehensive detection technique and has potential for pesticide residue screening in fruits and vegetables.

Graphical Abstract

Keywords

UHPLC/ESI Q-Orbitrap Pesticide residues Multiplexing data-independent acquisition (mDIA) Variable data-independent acquisition (vDIA) nDATA 

Notes

Acknowledgements

The authors would like to acknowledge the United States Environmental Protection Agency National Pesticide Standard Repository for providing some of the pesticide standards required to build the pesticide compound database. The work was a result of a collaborative research agreement between the Canadian Food Inspection Agency and the United States Food and Drug Administration.

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.

Supplementary material

216_2019_1581_MOESM1_ESM.pdf (644 kb)
ESM 1 (PDF 643 kb)

References

  1. 1.
    Health Canada. Maximum residue limits for pesticides. http://pr-rp.hc-sc.gc.ca/mrl-lrm/index-eng.php. Accessed 14 Jan 2019.
  2. 2.
    US Environmental Portection Agency. Regulation of Pesticide Residues on Food. Maximum residue limits for pesticides. https://www.epa.gov/pesticide-tolerances. Accessed 14 Jan 2019.
  3. 3.
    Regulation (EC) No 396/2005 of the European Parliament and of the Council of 23 February 2005 on maximum residue levels of pesticides in or on food and feed of plant and animal origin and amending Council Directive 91/414/EEC. Off J Eur Union 2005; L70:1–16.Google Scholar
  4. 4.
  5. 5.
    Codex Pesticides Residues in Food Online Database. Maximum residue limits. http://www.fao.org/fao-who-codexalimentarius/codex-texts/dbs/pestres/en/. Accessed 14 Jan 2019.
  6. 6.
    Alder L, Greulich K, Kempe G, Vieth B. Residue analysis of 500 high priority pesticides: better by GC-MS or LC-MS/MS? Mass Spectrom Rev. 2006;25:838–65.CrossRefGoogle Scholar
  7. 7.
    Soriano JM, Jimenez B, Font G, Molto JC. Analysis of carbamate pesticides and their metabolites in water by solid phase extraction and liquid chromatography: a review. Crit Rev Anal Chem. 2001;31:19–52.CrossRefGoogle Scholar
  8. 8.
    Reinholds I, Pugajeva I, Bartkevics V. A reliable screening of mycotoxins and pesticide residues in paprika using ultra-high performance liquid chromatography coupled to high resolution Orbitrap mass spectrometry. Food Control. 2016;60:683–9.CrossRefGoogle Scholar
  9. 9.
    Martínez-Domínguez G, Romero-González R, Garrido Frenich A. Multi-class methodology to determine pesticides and mycotoxins in green tea and royal jelly supplements by liquid chromatography coupled to Orbitrap high resolution mass spectrometry. Food Chem. 2016;197:907–15.CrossRefGoogle Scholar
  10. 10.
    Zomer P, Mol HGJ. Simultaneous quantitative determination, identification and qualitative screening of pesticides in fruits and vegetables using LC-Q-Orbitrap™-MS. Food Addit Contam A. 2015;32(10):1628–36.CrossRefGoogle Scholar
  11. 11.
    Del Mar Gómez-Ramos M, Rajski Ł, Heinzen H, Fernández-Alba AR. Liquid chromatography Orbitrap mass spectrometry with simultaneous full scan and tandem MS/MS for highly selective pesticide residue analysis. Anal Bioanal Chem. 2015;407:6317–26.CrossRefGoogle Scholar
  12. 12.
    Wang J, Chow W, Chang J, Wong JW. 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. J Agric Food Chem. 2014;62:10375–91.CrossRefGoogle Scholar
  13. 13.
    Wang J, Chow W, Leung D, Chang J. Application of ultrahigh-performance liquid chromatography and electrospray ionization quadrupole orbitrap high-resolution mass spectrometry for determination of 166 pesticides in fruits and vegetables. J Agric Food Chem. 2012;60:12088–104.CrossRefGoogle Scholar
  14. 14.
    CAC/GL 90-2017, Guidelines on perforamnce criteria for methods of analysis for the determiantion of pesticide residues in food and feed. http://www.fao.org/fao-who-codexalimentarius/sh-proxy/fr/?lnk=1&url=https%253A%252F%252Fworkspace.fao.org%252Fsites%252Fcodex%252FStandards%252FCAC%2BGL%2B90-2017%252FCXG_090e.pdf. FAO/WHO Codex Alimentarius International Food Standards. Accessed on June 27, 2018.Google Scholar
  15. 15.
    European Union. Guidance document on analytical quality control and method validation procedures for pesticides residues analysis in food and feed. SANTE/11813/2017 Supersedes SANTE/11945/2015 Implemented by 01/01/2018 https://eceuropaeu/food/sites/food/files/plant/docs/pesticides_mrl_guidelines_wrkdoc_2017-11813pdf. Accessed on June 16, 2018.Google Scholar
  16. 16.
    Mezcua M, Malato O, Garcia-Reyes JF, Molina-Diaz A, Fernandez-Alba AR. Accurate-mass databases for comprehensive screening of pesticide residues in food by fast liquid chromatography time-of-flight mass spectrometry. Anal Chem. 2009;81:913–29.CrossRefGoogle Scholar
  17. 17.
    López MG, Fussell RJ, Stead SL, Roberts D, McCullagh M, Rao R. Evaluation and validation of an accurate mass screening method for the analysis of pesticides in fruits and vegetables using liquid chromatography-quadrupole-time of flight-mass spectrometry with automated detection. J Chromatogr A. 2014;1373:40–50.CrossRefGoogle Scholar
  18. 18.
    Mol HGJ, Zomer P, De Koning M. Qualitative aspects and validation of a screening method for pesticides in vegetables and fruits based on liquid chromatography coupled to full scan high resolution (Orbitrap) mass spectrometry. Anal Bioanal Chem. 2012;403:2891–908.CrossRefGoogle Scholar
  19. 19.
    Wang J, Chow W, Chang J, Wong JW. Development and validation of a qualitative method for target screening of 448 pesticide residues in fruits and vegetables using UHPLC/ESI Q-Orbitrap based on data independent acquisition and compound database. J Agric Food Chem. 2017;65:473–93.CrossRefGoogle Scholar
  20. 20.
    Lehotay SJ, Mastovska K, Lightfield AR. Use of buffering and other means to improve results of problematic pesticides in a fast and easy method for residue analysis of fruits and vegetables. J AOAC Int. 2005;88:615–29.Google Scholar
  21. 21.
    Wong JW, Wang J, Chow W, Carlson R, Jia Z, Zhang K, et al. Perspectives on liquid chromatography-high resolution mass spectrometry for pesticide screening in foods. J Agric Food Chem. 2018;66:9573–81.CrossRefGoogle Scholar
  22. 22.
    Turnipseed SB, Storey JM, Wu IL, Gieseker CM, Hasbrouck NR, Crosby TC, et al. Application and evaluation of a high-resolution mass spectrometry screening method for veterinary drug residues in incurred fish and imported aquaculture samples. Anal Bioanal Chem. 2018;410:5529–44.CrossRefGoogle Scholar
  23. 23.
    Wang J, Leung D, Chow W, Chang J, Wong JW. Target screening of 105 veterinary drug residues in milk using UHPLC/ESI Q-Orbitrap multiplexing data independent acquisition. Anal Bioanal Chem. 2018;410:5373–89.CrossRefGoogle Scholar

Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2019

Authors and Affiliations

  1. 1.Calgary LaboratoryCanadian Food Inspection AgencyCalgaryCanada
  2. 2.Center for Food Safety and Applied NutritionUS Food and Drug AdministrationCollege ParkUSA
  3. 3.ThermoFisher ScientificSan JoseUSA
  4. 4.Henan University of TechnologyZhengzhouChina

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