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Determination of pyrimethanil and kresoxim-methyl in soils by headspace solid-phase microextraction and gas chromatography-mass spectrometry

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Abstract

A method using headspace solid-phase microextraction (HS-SPME) then gas chromatography–mass spectrometry with selected ion monitoring (GC–MS, SIM) has been developed for determination of trace amounts of the fungicides pyrimethanil and kresoxim-methyl in soil and humic materials. Both fungicides were extracted on to a fused-silica fibre coated with 85 μm polyacrylate (PA). Response-surface methodology was used to optimise the experimental conditions. For soil samples the linear dynamic range of application was 0.004–1.000 μg g−1 for pyrimethanil and 0.013–1.000 μg g−1 for kresoxim-methyl. The detection limits were 0.001 μg g−1 and 0.004 μg g−1 for pyrimethanil and kresoxim-methyl, respectively. HP-SPME–GC–MS analysis was highly reproducible—relative standard deviations (RSD) were between 6.7 and 12.2%. The method was validated by analysis of spiked matrix samples and used to investigate the presence of pyrimethanil and kresoxim-methyl above the detection limits in soil and humic materials.

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References

  1. Kjolholt J (1985) J Chromatogr A 325:231

    Article  Google Scholar 

  2. Veningerová M, Parchar V, Kovacicová J, Uhnák J (1997) J Chromatogr A 774:333

    Article  PubMed  Google Scholar 

  3. Koinecke A, Kreusig R, Bahadir M (1997) J Chromatogr A 786:155

    Article  CAS  Google Scholar 

  4. López-Avila V, Charan C (1994) Trends Anal Chem 13:118

    Article  Google Scholar 

  5. Van der Velde E, De Haan W, Liem A (1992) J Chromatogr A 626:135

    Article  Google Scholar 

  6. Conte E, Milani R, Morali G, Abballe F (1997) J Chromatogr A 765:121

    Article  CAS  Google Scholar 

  7. Popp P, Keil P, Moder M, Paschke A, Thuss U (1997) J Chromatogr A 774:203

    Article  Google Scholar 

  8. Molins C, Hogendoorn E, Dijkman E, Heusinkveld H, Baumann R (2000) J Chromatogr A 869:487

    Article  CAS  PubMed  Google Scholar 

  9. Papadakis E, Papadopoulou-Mourkidou E (2002) J Chromatogr A 962:9

    Article  CAS  PubMed  Google Scholar 

  10. Bouaid A, Ramos L, González M, Fernández P, Cámara C (2001) J Chromatogr A 939:13

    Article  CAS  PubMed  Google Scholar 

  11. Navalón A, Prieto A, Araujo L, Vílchez J-L (2001) Chromatographia 54:377

    Google Scholar 

  12. Zang Z, Yang M, Pawliszyn J (1994) Anal Chem 66:844A

    CAS  Google Scholar 

  13. Boyd-Boland A, Pawliszyn J (1995) J Chromatogr A 704:163

    CAS  Google Scholar 

  14. Hernández F, Beltrán J, López F, Gaspar J (2000) Anal Chem 72:2313

    CAS  PubMed  Google Scholar 

  15. Ng W, Teo M, Laksi H (1999) Fresenius J Anal Chem 363:673

    CAS  Google Scholar 

  16. Doong R, Liao P (2001) J Chromatogr A 918:177

    Article  CAS  PubMed  Google Scholar 

  17. Tomlin C (1994) The pesticide manual: a world compendium, British crop protection council, 10th edn. Croydon, p 885

    Google Scholar 

  18. De Liñan C (2000) Vademecum de productos fitosanitarios y nutricionales, Ed. Agrotécnicas, 16th edn. Madrid, p 142

  19. Cabras P, Angioni A, Garau V, Minelli E (1997) J AOAC Int 80:867

    CAS  PubMed  Google Scholar 

  20. Cabras P, Angioni A, Garau V, Pirisi F, Brandolini V (1998) J AOAC Int 81:1185

    CAS  PubMed  Google Scholar 

  21. Wong J, Halverson C (1999) Am J Enol Viticulture 50:435

    CAS  Google Scholar 

  22. Navickiene S, Ribeiro M-L (2001) J Sep Sci 24:470

    Article  CAS  Google Scholar 

  23. Navalón A, Prieto A, Araujo L, Vílchez J-L (2002) J Chromatogr A 975:355

    PubMed  Google Scholar 

  24. Otto M (1999) Chemometrics. Wiley–VCH, Weinheim

  25. Aguilar C, Peñalver A, Pocurull E, Ferré J, Borrull F, Marcé R-M (1999) J Chromatogr A 844:425

    Article  CAS  PubMed  Google Scholar 

  26. Salafranca J, Domeño C, Fernandez C, Nerin C (2003) Anal Chim Acta 477:257

    Article  CAS  Google Scholar 

  27. García-Campaña A, Cuadros-Rodríguez L, Lupiañez A, Alés-Barrero F, Román-Ceba M (1997) Anal Chim Acta 348:237

    Article  Google Scholar 

  28. Analytical Methods Committee (1994) Analyst 119:2363

    Article  Google Scholar 

  29. Pawliszyn J (1997) Solid phase microextraction: theory and practice. Wiley–VCH Inc, New York

    Google Scholar 

  30. Miller J-C, Miller J-N (1993) Statistics for chemical analysis. Addison-Wesley Iberoamericana, Wilmington

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Acknowledgements

The authors are grateful to the University of Zulia (Venezuela) for doctoral fellowships to A. Prieto and L. Araujo.

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Author notes

  1. Avismelsi Prieto

    Present address: Faculty of Agronomy, University of Zulia, PO Box 6610, Maracaibo, Venezuela

  2. Lilia Araujo

    Present address: Faculty of Engineering, University of Zulia, 10259, Maracaibo, Venezuela

Authors and Affiliations

  1. Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Avda. Fuentenueva s/n, 18071, Granada, Spain

    Alberto Navalón & José Luis Vílchez

Authors
  1. Alberto Navalón
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  2. Avismelsi Prieto
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  3. Lilia Araujo
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  4. José Luis Vílchez
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Corresponding author

Correspondence to José Luis Vílchez.

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Navalón, A., Prieto, A., Araujo, L. et al. Determination of pyrimethanil and kresoxim-methyl in soils by headspace solid-phase microextraction and gas chromatography-mass spectrometry. Anal Bioanal Chem 379, 1100–1105 (2004). https://doi.org/10.1007/s00216-004-2685-z

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  • DOI: https://doi.org/10.1007/s00216-004-2685-z

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