, Volume 53, Supplement 1, pp S361–S365 | Cite as

Analysis of pesticides volatilised from plants and soil by headspace solid-phase microextraction and gas chromatography

  • J. Castro
  • R. A. Pérez
  • C. Sánchez-Brunete
  • J. L. Tadeo
Originals Gas Chromatography


Pesticides volatilised from plants and soil were determined by headspace SPME and gas chromatography with electron-capture and mass spectrometric detection. SPME analyses were carried out with polydimethylsiloxane (PDMS) and polyacrylate (PA) fibres. A mixture of endosulfan, chlorpyrifos, lindane and pendimethalin was used in these assays. Fortified soil and plant samples were maintained at 30°C, for 2 h and 1 h, respectively, before SPME sampling. Pesticides were extracted by SPME by inserting the sheathed fibre through the cap and exposing it to the headspace for 1 h.

GC-ECD analysis was performed after thermal desorption of pesticides from the fibre for 5 minutes. Pesticide identity was confirmed by mass spectrometry operating in the electron impact mode (El). The SPME fibres assayed gave good results, the response obtained with the PDMS fibre being somewhat better in the concentration range studied. Detection limits for the compounds studied varied from 1 to 8 ng L−1.

Key Words

Gas chromatography SPME Pesticides Plants and soil 


  1. [1]
    Pawliszyn, J.,Solid Phase Microextraction-Theory and Practice, Wiley-VCH, New York1997.Google Scholar
  2. [2]
    Djozan, Dj.; Assadi, Y.Chromatographia 1997,45, 183–189.Google Scholar
  3. [3]
    Matisová, E.; Sedláková, J.; Slezácková, M.; Welsh, T.J. High Resol. Chromatogr. 1999,22, 109–115.CrossRefGoogle Scholar
  4. [4]
    Potter, D.W.; Pawliszyn,J. Environ. Sci. Technol. 1994,28, 298–305.CrossRefGoogle Scholar
  5. [5]
    Beltran, J.; Lopez, F.J.; Cepria, O.; Hernandez, F.J. Chromatogr. A. 1998,808, 257–263.CrossRefGoogle Scholar
  6. [6]
    Young, R.; Lopez-Avila, V.J. High Resol. Chromatogr. 1996,19, 247–256.CrossRefGoogle Scholar
  7. [7]
    Natangelo, M.; Tavazzi, S.; Fanelli, R.; Benfenati, E.J. Chromatogr. A.1999,859, 193–201.CrossRefGoogle Scholar
  8. [8]
    Volmer, D.A.; Hui, J.P.M.Arch. Environ. Contam. Toxicol. 1998,35, 1–7.CrossRefGoogle Scholar
  9. [9]
    Eisert, R.; Levsen, K.Fresenius J. Anal. Chem. 1995,351, 555–562.CrossRefGoogle Scholar
  10. [10]
    Magdic, S.; Boyd-Boland, A.; Jinno, K.; Pawliszyn, J.B.J. Chromatogr. A.1996,736, 219–228.CrossRefGoogle Scholar
  11. [11]
    Volante, M.; Pontello, M.; Valoti, L.; Cattaneo, M.; Bianchi, M.; Colzani, L.Pest Management Science.2000, 56, 618–636.CrossRefGoogle Scholar
  12. [12]
    Hu, R.; Hennion, B.; Urruty, L.; Montury, M.Food Additives and Contaminants.1999,16, 111–117.CrossRefGoogle Scholar
  13. [13]
    Volante, M.; Cattaneo, M.; Bianchi, M.; Zoccola, G.J. Environ. Sci. Health. 1998,33, 279–292.Google Scholar
  14. [14]
    Fromberg, A.; Nilsson, T.; Larsen, B.R.; Montanarella, L.; Faccheti, S.; Madsen, J.O.J. Chromatogr. A.1996,746, 71–81.CrossRefGoogle Scholar
  15. [15]
    James, K.J.; Stack, M.A.J. High Resol. Chromatogr. 1996,19, 515–519.CrossRefGoogle Scholar
  16. [16]
    Lee, M.-R.; Yeh, Y.-C.; Hsiang, W.-S.; Hwang, B.-H.J. Chromatogr. A.1998,806, 317–324.CrossRefGoogle Scholar
  17. [17]
    Chai, M.; Tang, Y.-Z.Inter. J. Environ. Anal. Chem. 1998,72, 77–82.Google Scholar
  18. [18]
    Llompart, M.; Li, K.; Fingas, M.J. Chromatogr. A.1998,824, 53–61.CrossRefGoogle Scholar
  19. [19]
    Rüdel, H.Chemosphere. 1997,35, 143–152.CrossRefGoogle Scholar
  20. [20]
    Eisert, R.; Levsen, K.J. Chromatogr. A. 1996, 143–157.Google Scholar
  21. [21]
    Miyahara, M.; Okada, Y.; Takeda, H.; Aoki, G.; Kobayashi, A.; Saito, Y.J. Agric. Food Chem. 1994,42, 2795–2802.CrossRefGoogle Scholar
  22. [22]
    Sannino, A.; Mambriani, P.; Bandini, M.; Bolzoni, L.J. AOAC Intern. 1996,79, 1434–1446.Google Scholar
  23. [23]
    Papadopoulou-Mourkidou, E.; Patsias, J.; Kotopoulou, A.J. AOAC Intern. 1997,80, 447–454.Google Scholar
  24. [24]
    García-Valcarcel, A.I.; Sánchez-Brunete, C.; Martínez, L.; Tadeo, J.L.J. Chromatogr. A.1996,719, 113–119.CrossRefGoogle Scholar
  25. [25]
    Barltelt, R.J.Anal. Chem. 1997,69, 364–372.CrossRefGoogle Scholar

Copyright information

© Friedr. Vieweg & Sohn Verlagsgesellschaft mbH 2001

Authors and Affiliations

  • J. Castro
    • 1
  • R. A. Pérez
    • 2
  • C. Sánchez-Brunete
    • 1
  • J. L. Tadeo
    • 1
  1. 1.Departamento de Uso Sostenible del Medio Natural (INIA)MadridSpain
  2. 2.Departamento de Protección Vegetal (INIA)MadridSpain

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