, Volume 59, Issue 5–6, pp 321–327 | Cite as

Validation of a Gas Chromatographic–Tandem Mass Spectrometric Method for Analysis of Pesticide Residues in Six Food Commodities. Selection of a Reference Matrix for Calibration

  • J. L. Martínez Vidal
  • F. J. Arrebola
  • A. Garrido Frenich
  • J. Martínez Fernández
  • M. Mateu-Sanchez


A gas chromatographic–tandem mass spectrometric (GC–MS–MS) method for analysis of 30 multi-class pesticide residues in four vegetables (cucumber, marrow, pepper, and eggplant) and two fruits (melon and watermelon) has been developed and validated. The performance characteristics linearity, detection limit (LOD), quantification limit (LOQ), precision, and recovery were studied. The effect of the matrix on the calibration step was studied by comparing calibration curves and recoveries for each food commodity. Two different food commodities, cucumber and watermelon, were selected as potential reference matrixes for the target vegetables and fruits, respectively.


Gas chromatography MS MS Matrix-matched calibration Pesticide analysis Vegetables 


Unable to display preview. Download preview PDF.

Unable to display preview. Download preview PDF.


  1. Order 93/58/EEC of Council, Official Bulletin of European Communities, Bureau of Official Publications of European CommunitiesGoogle Scholar
  2. Royal Order 280/1994 Annex of Official Spanish Bulletin 58, Official Spanish Bulletin Bureau. Madrid, SpainGoogle Scholar
  3. Commission of the European Communities (1999) White Paper on Food Safety. Brussels, BelgiumGoogle Scholar
  4. Martínez Vidal JL, Arrebola FJ, Mateu-Sánchez M (2002) J Chromatogr A 959: 203–213Google Scholar
  5. Martínez Vidal JL, Arrebola FJ, Mateu-Sánchez M (2002) Chromatographia 56: 475–482Google Scholar
  6. Martínez Vidal JL, Arrebola FJ, Mateu-Sánchez M (2002) Rapid Commun Mass Spectrom 16:1106–1115CrossRefPubMedGoogle Scholar
  7. Amirav A, Jing H (1998) J Chromatogr A 814:133–150CrossRefPubMedGoogle Scholar
  8. Schachterle S, Feigel C (1996) J Chromatogr A 754:411–422CrossRefPubMedGoogle Scholar
  9. Arrebola FJ, Martínez Vidal JL, Fernández Gutiérrez A, Akhtar MH (1999) Anal Chim Acta 401:45–54CrossRefGoogle Scholar
  10. McLafferty FW (1983) In: Tandem mass spectrometry. Wiley, New YorkGoogle Scholar
  11. Busch KL, Glish GL, McLuckey SA (1988) In: Mass spectrometry; techniques and applications of tandem mass spectrometry. VCH, New YorkGoogle Scholar
  12. Lee MR, See J, Hsiang WS, Chen CM (1997) J Chromatogr A 775:267–274CrossRefGoogle Scholar
  13. Agüera A, Piedra L, Hernando MD, Fernández-Alba AR, Contreras M (2000) Analyst 125:1397–1402CrossRefPubMedGoogle Scholar
  14. Hernando MD, Agüera A, Fernández-Alba AR, Piedra L, Contreras M (2001) Analyst 126:46–51CrossRefGoogle Scholar
  15. Sheridan RS, Meola JR (1999) J AOAC Int 82:982–990PubMedGoogle Scholar
  16. Pylypiw HM Jr (1993) J Assoc Off Anal Chem 76:1369–1373Google Scholar
  17. Fillion J, Hindle R, Lacroix M, Selwyn J (1995) J AOAC Int 78:1252–1266Google Scholar
  18. General Inspectorate for Health Protection, Ministry of Public Health, Welfare and Sports (1996) Analytical methods for pesticide residues in foodstuffs (3rd edn). Amsterdam, The NetherlandsGoogle Scholar
  19. Erney DR, Guillespie AM, Gilvydis DM, Poole CF (1993) J Chromatogr A 638:57–63CrossRefGoogle Scholar
  20. Hajšlová J, Holadová K, Kocourek V, Poutska J, Godula M, Cuhra P, Kempný M (1998) J Chromatogr A 800:283–295CrossRefGoogle Scholar
  21. Johnson PD, Rimmer DA, Brown RH (1997) J Chromatogr A 765:3–11CrossRefGoogle Scholar
  22. Lehotay SJ, Eller KI (1995) J AOAC Int 78:821–830PubMedGoogle Scholar
  23. Schenk FJ, Lehotay SJ (2000) J Chromatogr A 868:51–61Google Scholar
  24. Hill ARC, Reynolds SL (1999) Analyst 124:953–958CrossRefPubMedGoogle Scholar
  25. Egea González FJ, Hernández Torres ME, Almansa López E, Cuadros-Rodríguez L, Martínez Vidal JL (2002) J Chromatogr A 966:155–165CrossRefPubMedGoogle Scholar
  26. National Institute of Standards and Technology (1998) Standard Reference Program, The NIST Mass Spectral Library V. 1.6d, USAGoogle Scholar
  27. Pfleger K, Maurer HH, Weber A (1992) Mass spectral and GC data of drugs, poisons, pesticides, pollutants and their metabolites, 2nd revised and enlarged edition. VCH, Weinheim, GermanyGoogle Scholar
  28. Nomenclature, symbols, units and their usage in spectrochemical analysis II (1978) Spectrochim Acta B 33:242–245Google Scholar
  29. Vandeginste BGM, Massart DL, Buydens LMC, De Jong S, Lewi PJ, Smeyers-Verbeke J (1998) Handbook of chemometrics and qualimetrics: part B. Elsevier, Amsterdam, The NetherlandsGoogle Scholar

Copyright information

© Friedr. Vieweg&Sohn Verlagsgesellschaft mbH 2004

Authors and Affiliations

  • J. L. Martínez Vidal
    • 1
  • F. J. Arrebola
    • 1
  • A. Garrido Frenich
    • 1
  • J. Martínez Fernández
    • 2
  • M. Mateu-Sanchez
    • 2
  1. 1.Department of Analytical ChemistryUniversity of AlmeríaAlmeríaSpain
  2. 2.Pesticide Residue LaboratoryC.U.A.MEl Ejido AlmeríaSpain

Personalised recommendations