Determination of organophosphorus pesticides in pakchoi samples by headspace solid-phase microextraction coupled with gas chromatography using home-made fiber


A home-made sol-gel-derived co-poly (hydroxy-terminated silicone divinylbenzene) (OH-TSO/DVB) coating fiber has firstly been applied for headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography (GC)—nitrogen-phosphorus detector (NPD) to determine five organophosphorus pesticides (OPPs) in pakchoi samples. The following parameters influencing on the extraction efficiency of HS-SPME were optimized statistically: extraction temperature, extraction time, ionic strength, constant agitation, effect of sample matrix, desorption temperature, and desorption time. Compared with commercial available fibers and OH-TSO SPME fiber, this fiber showed statistically better enrichment capability for these pesticides. For the developed HS-SPME-GC method, it was found that the linearity was all two orders of magnitude, with the limits of detection (LOD) ranging from 0.007 to 0.07 ng g−1, and relative standard deviations (RSD) varying between 4.1 and 8.7% (n = 5). Recoveries of spiked pakchoi samples ranged from 80.74 to 101.47% for every pesticide at each investigated concentration. Overall, it indicated that the obtained method is a validated and accurate procedure for determination of OPPs in pakchoi samples.

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  1. 1.

    Beltran J, López FJ, Hernández F (2000) J Chromatogr A 885:389–404

    Article  CAS  Google Scholar 

  2. 2.

    Tahboub YR, Zaater MF, Al-Talla ZA (2005) J Chromatogr A 1098:150–155

    Article  CAS  Google Scholar 

  3. 3.

    Pagliuca G, Gazzotti T, Zironi E, Sticca P (2005) J Chromatogr A 1071:67–70

    Article  CAS  Google Scholar 

  4. 4.

    Gonçalves C, Carvalho JJ, Azenha MA, Alpendurada MF (2006) J Chromatogr A 1110:6–14

    Article  Google Scholar 

  5. 5.

    Barnabas IJ, Dean JR, Hitchen SM, Owen SP (1994) Anal Chim Acta 291:261–267

    Article  CAS  Google Scholar 

  6. 6.

    Zuin VG, Yariwake JH, Bicchi C (2003) J Chromatogr A 985:159–166

    Article  CAS  Google Scholar 

  7. 7.

    Arthur CL, Pawliszyn J (1990) Anal Chem 62:2145–2148

    Article  CAS  Google Scholar 

  8. 8.

    Campillo N, Peñalver R, Aguinaga N, Hernández-Córdoba M (2006) Anal Chim Acta 562:9–15

    Article  CAS  Google Scholar 

  9. 9.

    Lambropoulou DA, Albanis TA (2001) J Chromatogr A 922:243–255

    Article  CAS  Google Scholar 

  10. 10.

    Farajzadeh MA, Hatami M (2004) Chromatographia 59:259–262

    CAS  Google Scholar 

  11. 11.

    Hernández F, Pitarch E, Beltran J, López FJ (2002) J Chromatogr B 769:65–77

    Article  Google Scholar 

  12. 12.

    Bouaid A, Ramos L, Gonzalez MJ, Fernández P, Cámara C (2001) J Chromatogr A 939:13–21

    Article  CAS  Google Scholar 

  13. 13.

    Simplício AL, Boas LV (1999) J Chromatogr A 833:35–42

    Article  Google Scholar 

  14. 14.

    Livage J, Henry M, Sanchez CJ (1988) Solid State Chem 18:259–341

    Article  CAS  Google Scholar 

  15. 15.

    Chong SL, Wang D, Hayes JD, Wilhite BW, Malik A (1997) Anal Chem 69:3889–3898

    Article  CAS  Google Scholar 

  16. 16.

    Yu JX, Wu CY, Xing J (2004) J Chromatogr A 1036:101–111

    Article  CAS  Google Scholar 

  17. 17.

    Cai LS, Gong SL, Chen M, Wu CY (2006) Anal Chim Acta 559:89–96

    Article  CAS  Google Scholar 

  18. 18.

    Zeng ZR, Qiu WL, Huang ZF (2001) Anal Chem 73:2429–2436

    Article  CAS  Google Scholar 

  19. 19.

    Yang M, Zeng ZR, Qiu WL, Wang YL (2002) Chromatographia 56:73–80

    Article  CAS  Google Scholar 

  20. 20.

    Yun L (2003) Anal Chim Acta 486:63–72

    Article  CAS  Google Scholar 

  21. 21.

    Li XJ, Zeng ZR, Gao SZ, Li HB (2004) J Chromatogr A 1023:15–25

    Article  CAS  Google Scholar 

  22. 22.

    Liu MM, Zeng ZR, Wang CL, Tan YJ, Liu H (2003) Chromatographia 58:597–605

    CAS  Google Scholar 

  23. 23.

    Zhou FR, Li XJ, Zeng ZR (2005) Anal Chim Acta 538:63–70

    Article  CAS  Google Scholar 

  24. 24.

    Liu MM, Zeng ZR, Tian Y (2005) Anal Chim Acta 540:341–353

    Article  CAS  Google Scholar 

  25. 25.

    Li XJ, Gong SL, Zeng ZR (2005) Chromatographia 62:519–525

    Article  CAS  Google Scholar 

  26. 26.

    Cha DM, Liu MM, Zeng ZR, Cheng DE, Zhan GQ (2006) Anal Chim Acta 572:47–54

    Article  CAS  Google Scholar 

  27. 27.

    Zhou JJ, Zeng ZR (2006) Anal Chim Acta 556:400–406

    Article  CAS  Google Scholar 

  28. 28.

    Li XJ, Zeng ZR, Chen Y, Xu Y (2004) Talanta 63:1013–1019

    Article  CAS  Google Scholar 

  29. 29.

    Dong CZ, Zeng ZR, Li XJ (2005) Talanta 66:721–727

    Article  CAS  Google Scholar 

  30. 30.

    Ai J (1998) Anal Chem 70:4822–4826

    Article  CAS  Google Scholar 

  31. 31.

    Dong CZ, Zeng ZR, Yang M (2005) Water Res 39:4204–4210

    Article  CAS  Google Scholar 

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This work was kindly supported by a Key Technology Grant of Hubei Province (Grant No. 2003AA207B06) and Science Research Foundation of Wuhan University of Technology (Grant No. XJJ2002062).

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Correspondence to Zhao-Rui Zeng.

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Wang, YL., Zeng, ZR., Liu, MM. et al. Determination of organophosphorus pesticides in pakchoi samples by headspace solid-phase microextraction coupled with gas chromatography using home-made fiber. Eur Food Res Technol 226, 1091–1098 (2008).

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  • Co-poly (hydroxy-terminated silicone divinylbenzene) coating
  • Organophosphorus pesticides
  • Pakchoi samples
  • Headspace solid-phase microextraction
  • Gas chromatography