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Further improvements in pesticide residue analysis in food by applying gas chromatography triple quadrupole mass spectrometry (GC-QqQ-MS/MS) technologies

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Abstract

Nowadays, the control of pesticide residues in food is well established. The capacity of triple quadrupole technology to satisfy the current food regulations has been demonstrated. However, the permanent high demand of consumers for more sensitive and faster testing is driving the development of improved analytical methodologies that increase the performances of sensitivity and robustness and reduce the analysis time. In this work, the feasibility of decreasing the run time to 12.4 min by modifying the oven temperature program, for a multiresidue method covering 203 pesticides, was evaluated. Satisfactory sensitivity results were achieved by reaching a limit of quantitation of 2 μg kg−1 for a great variety of fruits and vegetables. The validated method based on updated GC-QqQ-MS/MS has confirmed the abovementioned challenges with adequate robustness by its application to routine analyses for 69 real samples. The proposed method can represent great benefit for laboratories as it allows increasing samples throughput. It is also very useful for risk assessment studies, where the needs of low reporting limits and very wide analytical scope are necessary.

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References

  1. Uclés S, et al. Validation of a multiclass multiresidue method and monitoring results for 210 pesticides in fruits and vegetables by gas chromatography-triple quadrupole mass spectrometry. J Environ Sci Health. 2014;49(8):557–68.

    Article  CAS  Google Scholar 

  2. Lee J, et al. Rapid and simultaneous analysis of 360 pesticides in brown rice, spinach, orange, and potato using micropore GC-MS/MS. J Agric Food Chem. 2017;65(16):3387–95.

    Article  CAS  PubMed  Google Scholar 

  3. Walorczyk S, Kopeć I, Szpyrka E. Pesticide residue determination by gas chromatography-tandem mass spectrometry as applied to food safety assessment on the example of some fruiting vegetables. Food Anal Methods. 2016;9(5):1155–72.

    Article  Google Scholar 

  4. Machado I, et al. Determination of pesticide residues in globe artichoke leaves and fruits by GC–MS and LC–MS/MS using the same QuEChERS procedure. Food Chem. 2017;227:227–36.

    Article  CAS  PubMed  Google Scholar 

  5. Sawant D, et al. Fast gas chromatography with tandem mass spectrometry analysis of selected persistent organic pollutants and organophosphorus and synthetic pyrethroid pesticides in Indian prawn (Fenneropenaeus indicus) in compliance with the EU-MRLs. J AOAC Int. 2017;100(3):610–5.

    Article  CAS  PubMed  Google Scholar 

  6. Silva AS, et al. A multiclass analytical method for pesticides determination in water using DLLME and GC-MS. Rev Virtual Quim. 2017;9(2):550–62.

    Google Scholar 

  7. Rai S, et al. A rapid method for the quantitative determination of 34 pesticides in nonalcoholic carbonated beverages using liquid-liquid extraction coupled to dispersive solid-phase cleanup followed by gas chromatography with tandem mass spectrometry. J AOAC Int. 2017;100(3):624–30.

    Article  CAS  PubMed  Google Scholar 

  8. Van Deursen MM, et al. Evaluation of time-of-flight mass spectrometric detection for fast gas chromatography. J Chromatogr A. 2000;878(2):205–13.

    Article  Google Scholar 

  9. Matisová E, Hrouzková S. Analysis of endocrine disrupting pesticides by capillary GC with mass spectrometric detection. Int J Environ Res Public Health. 2012;9(9):3166–96.

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  10. van Ysacker PG, et al. Electron capture detection in high speed narrow bore capillary gas chromatography: fast and sensitive analysis of PCBs and pesticides. J High Resolut Chromatgr. 1995;18(7):397–402.

    Article  Google Scholar 

  11. Dömötörová M, et al. Fast gas chromatography of polar and non-polar compounds with the on-column injection. Chem Anal. 2005;50(2):365–75.

    Google Scholar 

  12. Tanaka KM, Miyagawa H, Nakagawa K. Analysis time reduction using fast gas chromatography-mass spectrometry. J Anal Sci. 2001;17:885–6.

    Article  Google Scholar 

  13. Hada M, et al. Trace analysis of pesticide residues in water by high-speed narrow-bore capillary gas chromatography-mass spectrometry with programmable temperature vaporizer. J Chromatogr A. 2000;874(1):81–90.

    Article  CAS  PubMed  Google Scholar 

  14. Korenková E, Matisová E, Slobodník J. Study on the feasibility of coupling large-volume injection to fast gas chromatography with mass spectrometric detection for analysis of organochlorine pesticides. J Sep Sci. 2003;26(12–13):1193–7.

    Article  CAS  Google Scholar 

  15. Purdešová A, et al. Evaluation of calibration approaches for quantification of pesticide residues in surface water by SPE with small-size cartridges followed by fast GC-MS. J Anal Methods. 2013;5(13):3403–9.

    Article  CAS  Google Scholar 

  16. Cherta L, et al. Multiclass determination of 66 organic micropollutants in environmental water samples by fast gas chromatography-mass spectrometry. ABC. 2012;402(7):2301–14.

    CAS  Google Scholar 

  17. Kochman M, et al. Fast, high-sensitivity, multipesticide analysis of complex mixtures with supersonic gas chromatography-mass spectrometry. J Chromatogr A. 2002;974(1–2):185–212.

    Article  CAS  PubMed  Google Scholar 

  18. Hercegová A, et al. Fast gas chromatography with solid phase extraction clean-up for ultratrace analysis of pesticide residues in baby food. J Chromatogr A. 2005;1084(1–2):46–53.

    Article  CAS  PubMed  Google Scholar 

  19. Hercegová A, et al. Study on pesticide residues in apples, apple-based baby food, and their behaviour during processing using fast GC-MS multiresidue analysis. Int J Environ Anal Chem. 2007;87(13–14):957–69.

    Article  CAS  Google Scholar 

  20. Kirchner M, et al. Fast gas chromatography for pesticide residues analysis using analyte protectants. J Chromatogr A. 2008;1186(1–2):271–80.

    Article  CAS  PubMed  Google Scholar 

  21. Húšková R, Matisová E, Kirchner M. Fast GC-MS pesticide multiresidue analysis of apples. Chromatographia. 2008;68(SUPPL. 1):S49–55.

    Article  CAS  Google Scholar 

  22. Čajka T, Hajšlová J. Gas chromatography-high-resolution time-of-flight mass spectrometry in pesticide residue analysis: advantages and limitations. J Chromatogr A. 2004;1058(1–2):251–61.

    Article  Google Scholar 

  23. Patel K, et al. Analysis of pesticide residues in lettuce by large volume-difficult matrix introduction-gas chromatography-time of flight-mass spectrometry (LV-DMI-GC-TOF-MS). Analyst. 2003;128(10):1228–31.

    Article  CAS  PubMed  Google Scholar 

  24. Maštovská K, Lehotay SJ. Practical approaches to fast gas chromatography-mass spectrometry. J Chromatogr A. 2003;1000(1–2):153–80.

    Article  CAS  PubMed  Google Scholar 

  25. Klee MS, Blumberg LM. Theoretical and practical aspects of fast gas chromatography and method translation. J Chromatogr Sci. 2002;40(5):234–47.

    Article  CAS  PubMed  Google Scholar 

  26. Blumberg LM, Klee MS. Optimal heating rate in gas chromatography. JMS. 2000;12(9):508–14.

    CAS  Google Scholar 

  27. Vaclavik L, et al. Survey of mass spectrometry-based high-throughput methods in food analysis, in high-throughput analysis for food safety. 2014; 15–72.

  28. Woolt L, Decker D. Practical fast gas chromatography for contract laboratory program pesticide analyses. J Chromatogr Sci. 2002;40(8):434–40.

    Article  Google Scholar 

  29. Mondello L, et al. Ultra-fast essential oil characterization by capillary GC on 50 μm ID column. J Sep Sci. 2004;27(9):699–702.

    Article  CAS  PubMed  Google Scholar 

  30. McNair HM, Reed GL. Fast gas chromatography: the effect of fast temperature programming. JMS. 2000;12(6):351–5.

    CAS  Google Scholar 

  31. Martínez Vidal JL, et al. Trace determination of organotin compounds in water, sediment and mussel samples by low-pressure gas chromatography coupled to tandem mass spectrometry. RCM. 2003;17(18):2099–106.

    Google Scholar 

  32. Maštovská K, Hajšlová J, Lehotay SJ. Ruggedness and other performance characteristics of low-pressure gas chromatography-mass spectrometry for the fast analysis of multiple pesticide residues in food crops. J Chromatogr A. 2004;1054(1–2):335–49.

    PubMed  Google Scholar 

  33. Han L, Sapozhnikova Y, Lehotay SJ. Method validation for 243 pesticides and environmental contaminants in meats and poultry by tandem mass spectrometry coupled to low-pressure gas chromatography and ultrahigh-performance liquid chromatography. Food Control. 2016;66:270–82.

    Article  CAS  Google Scholar 

  34. Malato O, et al. Benefits and pitfalls of the application of screening methods for the analysis of pesticide residues in fruits and vegetables. J Chromatogr A. 2011;1218(42):7615–26.

    Article  CAS  PubMed  Google Scholar 

  35. European Commission DG-SANTE. Guidance document on analytical quality control and method validation procedures for pesticide residues analysis in food and feed, N.S. 2015.

  36. European Standard. Foods of plant origin—determination of pesticide residues using GC-MS and/or LC-MS/MS following acetonitrile extraction/partitioning and clean-up by dispersive SPE-QuEChERS-method. CSN EN 15662 2008.

  37. Furey A, et al. Ion suppression; a critical review on causes, evaluation, prevention and applications. Talanta. 2013;115:104–22.

    Article  CAS  PubMed  Google Scholar 

  38. EU pesticides database available at: http://www.ec.europa.eu.

  39. Anastassiades M, et al. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce. J AOAC Int. 2003;86(2):412–31.

    CAS  PubMed  Google Scholar 

  40. Shen CY, et al. Determination of 17 pyrethroid residues in troublesome matrices by gas chromatography/mass spectrometry with negative chemical ionization. Talanta. 2011;84(1):141–7.

    Article  CAS  PubMed  Google Scholar 

  41. Uclés A, et al. Application of zirconium dioxide nanoparticle sorbent for the clean-up step in post-harvest pesticide residue analysis. Talanta. 2015;144:51–61.

    Article  CAS  PubMed  Google Scholar 

  42. EURL-SRM, improvement of ethoxyquin recoveries by QuEChERS through the addition of ascorbic acid initiator/Institution: EURL-SRM version 1 (last update: 22 July 2014).

  43. PubChem database available at: https://www.ncbi.nlm.nih.gov/pccompound.

  44. Pesticides properties database PPDB available at: http://sitem.herts.ac.uk/aeru/ppdb/en/.

  45. Lozowicka B, Rutkowska E, Hrynko I. Simultaneous determination of 223 pesticides in tobacco by GC with simultaneous electron capture and nitrogen-phosphorous detection and mass spectrometric confirmation. Open Chem. 2015;13(1):1137–49.

    Article  CAS  Google Scholar 

  46. Uclés S, et al. Matrix interference evaluation employing GC and LC coupled to triple quadrupole tandem mass spectrometry. Talanta. 2017;174:72–81.

    Article  CAS  PubMed  Google Scholar 

  47. Lozano A, et al. Pesticide analysis in teas and chamomile by liquid chromatography and gas chromatography tandem mass spectrometry using a modified QuEChERS method: validation and pilot survey in real samples. J Chromatogr A. 2012;1268:109–22.

    Article  CAS  PubMed  Google Scholar 

  48. Ferrer C, et al. European Union proficiency tests for pesticide residues in fruit and vegetables from 2009 to 2016: overview of the results and main achievements. Food Control. 2017;82:101–13.

    Article  CAS  Google Scholar 

Download references

Acknowledgments

The authors acknowledge funding support from the European Commission, DG SANTE (Grant decision SI2.726352) and thank Joerg Riener from Agilent Technologies for his technical support.

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Correspondence to Amadeo R. Fernández-Alba.

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The authors declare no conflict of interest with any of the instruments or materials referred to in this work.

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Published in the topical collection Food Safety Analysis with guest editor Steven J. Lehotay.

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Hakme, E., Lozano, A., Uclés, S. et al. Further improvements in pesticide residue analysis in food by applying gas chromatography triple quadrupole mass spectrometry (GC-QqQ-MS/MS) technologies. Anal Bioanal Chem 410, 5491–5506 (2018). https://doi.org/10.1007/s00216-017-0723-x

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  • DOI: https://doi.org/10.1007/s00216-017-0723-x

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