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Gas chromatographic determination of selected pesticides in human serum by head-space solid-phase microextraction

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Summary

A simple and rapid method, employing head-space solid-phase microextraction then gas chromatography-mass spectrometry, has been developed for the simultaneous determination of nine organochlorine pesticides (α-HCH, hexachlorobenzene, lindane, endosulfan ether, α-endosulfan,p,p′-DDE,p,p′-DDD, endosulfan sulfate, andp,p′-DDT) and five organophosphorus pesticides (fonofos, parathion methyl, fenitrothion, chlorpyrifos, and ethion) in human serum. Sulfuric acid (9m, 50 μl), water (2 mL), and surrogate/internal standard solution (p,p′-DDE-D8, hexachlorobenzene-13C6, and fenitrothion D6; 50 μL) were added to the serum sample (1 mL) and the resulting solution was sampled by head-space SPME at 90°C for 30 min. Quantitation was performed by means of calibration curves prepared by use of serum, using areas relative to those of the surrogates. Precision was found to be better than 20% at three concentration levels assayed in the ng mL−1 range. The detection limits were in the range 0.1 to 6 ng mL−1 for all compounds.

Finally, application of the optimized procedure enabled the detection of some pesticides in serum samples obtained from agricultural workers. Hexachlorobenzene,p,p′-DDE, and chlorpyrifos were found most frequently in the samples analyzed.

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References

  1. Ameno, K.; Fuke, C.; Ameno, S.; Kiriu, T.; Ijiri, Y.J. Anal. Toxicol. 2000,13, 150–151.

    Google Scholar 

  2. Liu, J.; Suzuki, O.; Kumazaya, T.; Seno, H.Forensic Sci. Int. 1989,41, 67–72.

    Article  CAS  Google Scholar 

  3. Brock, J.W.; Burse, V.W.; Ashley, D.L.; Najam, A.R.; Green, V.E.; Korver, M.P.; Powell, M.K.; Hodge, C.C.; Needham, L.L.J. Anal. Toxicol. 1996, 20, 528–536.

    CAS  Google Scholar 

  4. Guardino, X.; Serra, C.; Obiols, J.; Rosell, M.G.; Berenguer, M.J.; López, F.; Brose, J.J. Chromatogr. A 1996,719, 141–147.

    Article  CAS  Google Scholar 

  5. Johnston, J.J.; Petty, E.E.; Volz, S.A.J. High Resol. Chromatogr. 1997,20, 405–409.

    Article  CAS  Google Scholar 

  6. Otero, R.; Santiago Silva, M.; Grimalt, J.O.J. Chromatogr. A 1997,778, 87–94.

    Article  CAS  Google Scholar 

  7. Waliszewski, S.M.; Szymczynski, G.A.Bull. Environ. Contam. Toxicol. 1991,46, 803–809.

    Article  CAS  Google Scholar 

  8. Gill, U.S.; Schwartz, H.M.; Wheatley, B.Chemosphere 1996,32, 1055–1061.

    Article  CAS  Google Scholar 

  9. Pauwels, A.; Wells, D.A.; Covaci, A.; Schepens, P.J.C.J. Chromatogr. B 1999,723, 117–125.

    CAS  Google Scholar 

  10. Atuma, S.S.; Aune, M.Bull. Environ. Contam. Toxicol. 1999,62, 8–15.

    Article  CAS  Google Scholar 

  11. Matos, C.; Ferreira, C.B.; Valente, D.S.; Rocha, J.M.; Noronha, M.I.J. Chromatogr. B 1998,716, 147–152.

    Google Scholar 

  12. Bucholski, K.A.; Begerow, J.; Winneke, G.; Dunemann, L.J. Chromatogr. A 1996,754, 479–485.

    Article  CAS  Google Scholar 

  13. Najam, A.R.; Korver, M.P.; Williams, C.C.; Burse, V.W.; Needham, L.L.J. AO AC Int. 1999,82, 177–185.

    CAS  Google Scholar 

  14. Arthur, C.L.; Pawliszyn, J.Anal. Chem. 1990,62, 2145–2148.

    Article  CAS  Google Scholar 

  15. Arthur, C.L.; Killam, L.M.; Buchholz, K.D.; Pawliszyn, J.; Berg, J.R.Anal. Chem. 1992,64, 1960–1966.

    Article  CAS  Google Scholar 

  16. Beltran, J.; López, F.J.; Cepria, O.; Hernández, F.J. Chromatogr. A 1998,808, 257–263.

    Article  CAS  Google Scholar 

  17. Beltran, J.; López, F.J.; Hernández, F.J. Chromatogr. A 2000,885, 389–404.

    Article  CAS  Google Scholar 

  18. Hernández, F.; Beltran, J.; López, F.J.; Gaspar, J.V.Anal. Chem. 2000,72, 2313–2322.

    Article  Google Scholar 

  19. Koster, E.H.M.; Hofman, N.S.K.; de Jong, G.J.;Chromatographia 1998,47, 678–684.

    Article  CAS  Google Scholar 

  20. Kumazawa, T.; Sato, K.; Seno, H.; Ishii, A.; Suzuki, O.Chromatographia 1996,43, 59–62.

    Article  CAS  Google Scholar 

  21. Krogh, M.; Grefslie, H.; Rasmussen, K.E.J. Chromatogr. B 1997,689, 357–364.

    CAS  Google Scholar 

  22. Ulrich, S.; Martens, J.J. Chromatogr. B 1998,696, 217–234.

    Google Scholar 

  23. Schaller, K.H., Angerer, J., Lehnert, G.Fresenius J. Anal. Chem. 1993,346, 830–832.

    Article  CAS  Google Scholar 

  24. Röhrig, L.; Püttmann, M.; Meisch, H.U.Fresenius J. Anal. Chem. 1998,361, 192–196.

    Article  Google Scholar 

  25. Namera, A.; Yashiki, M.; Nagasawa, N.; Iwasaki, Y.; Kojima, T.Forensic Sci. Int. 1997,88, 125–131.

    Article  CAS  Google Scholar 

  26. Lee, X.P.; Kumazawa, T.; Sato, K.; Suzuki, O.Chromatographia 1996,42, 135–140.

    Article  CAS  Google Scholar 

  27. Musshoff, F.; Junker, H.; Madea, B.Clin. Chem. Lab. Med. 1998,37, 639–642.

    Article  Google Scholar 

  28. Guan, F.; Watanabe, K.; Ishii, A.; Seno, H.; Kumazawa, T.; Hattori, H.; Suzuki, O.J. Chromatogr. B 1998,714, 205–213.

    Google Scholar 

  29. López, F.J., Pitarch, E.; Egea, S.; Beltran, J.; Hernández, F.Anal. Chim. Acta 2001,433, 217–226.

    Article  Google Scholar 

  30. Takekawa, K.; Oya, M.; Kido, A.; Suzuki, O.Chromatographia 1998,47, 209–214.

    Article  CAS  Google Scholar 

  31. Burse, V.W.; Head, S.L.; Korver, M.P.; McClure, P.C.; Donahue, J.F.; Needham, L.L.J. Anal. Toxicol. 1990,14, 137–142.

    CAS  Google Scholar 

  32. Beeson, M.D.; Driskell, W.J.; Barr, D.B.Anal. Chem. 1999,71, 3526–3530.

    Article  CAS  Google Scholar 

  33. Hill, R.H.; Shealy, D.B.; Head, S.L.; Willams, C.C.; Bailey, S.L.; Gregg, M.; Baker, S.E; Needham, L.L.J. Anal. Toxicol. 1995,19, 323–329.

    CAS  Google Scholar 

  34. Krauthacker, B.Bull. Environ. Contam. Toxicol. 1991,46, 797–802.

    Article  CAS  Google Scholar 

  35. Bjerregaard, P.; Hansen, J.C.Sci. Total Environ. 2000,245, 195–202.

    Article  CAS  Google Scholar 

  36. Kocan, A.; Petrík, J.; Drobná, B.; Chovancová, J.Chemosphere 1994,29, 2315–2325.

    Article  CAS  Google Scholar 

  37. Martínez Vidal, J.L.; Arrebola, F.J.; Fernández-Gutiérrez, A.; Rams, M.A.J. Chromatogr B 1998,719, 71–78.

    Google Scholar 

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Authors and Affiliations

  1. Analytical Chemistry, Experimental Sciences Department, University Jaume I, P.O. Box 8029, 12080, Castellón, Spain

    J. Beltran, E. Pitarch, S. Egea, F. J. López & F. Hernández

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  1. J. Beltran
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  2. E. Pitarch
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  3. S. Egea
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  4. F. J. López
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  5. F. Hernández
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Beltran, J., Pitarch, E., Egea, S. et al. Gas chromatographic determination of selected pesticides in human serum by head-space solid-phase microextraction. Chromatographia 54, 757–763 (2001). https://doi.org/10.1007/BF02492495

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  • DOI: https://doi.org/10.1007/BF02492495

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