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Multiresidue Analysis of Pesticides in Vegetables and Citrus Fruits by LC–MS–MS

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Abstract

In this work, an analytical multiresidue method using liquid chromatography tandem-mass spectrometry (LC–MS–MS) with triple quadrupole in selected reaction monitoring (SRM) mode for the simultaneous determination of 54 pesticides in vegetables (pepper and tomato) and citrus fruits (orange and lemon) has been developed. The procedure involves initial single phase extraction of sample with acetonitrile by agitation, followed by liquid–liquid partition aided by “salting out” process using NaCl. The average recovery by the LC–MS–MS method obtained for these compounds varied from 65.5 to 114.5% with a relative standard deviation between 2.3 and 8.3%. The method presents good linearity over the range assayed 10–500 μg L−1 (except famoxadone 50–1,000 μg L−1) and the detection limits for the pesticides studied varied from 0.03 to 14.9 μg kg−1. The proposed method was used to determine pesticide levels in vegetables and citrus fruit samples from different experimental orchards and greenhouses from the Region of Murcia.

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References

  1. Conacher HBS, Mes J (1993) Food Addit Contam 10:5–15

    CAS  Google Scholar 

  2. Luke M, Forberg JE, Masumoto HT (1975) J Assoc Off Anal Chem 58:1020–1026

    CAS  Google Scholar 

  3. Hsu RC, Biggs I, Saini NK (1991) J Agric Food Chem 39:1658–1666

    Article  CAS  Google Scholar 

  4. Rotich HK, Zhang ZY, Li JC (2003) Int J Environ Anal Chem 83:851–860

    Article  CAS  Google Scholar 

  5. Adou K, Bontoyan WR, Sweeney PJ (2001) J Agric Food Chem 49:4153–4160

    Article  CAS  Google Scholar 

  6. Andersson A, Palsheden H (1998) Livsmedelverket Rapport 17:9–41

    Google Scholar 

  7. Stan HJ (2000) J Chromatogr A 892:347–377

    Article  CAS  Google Scholar 

  8. Barriada-Pereira M, Gonzalez-Castro MJ, Muniategui-Lorenzo S, Lopez-Mahia P, Prada-Rodriguez D, Fernandez-Fernandez E (2005) Int J Environ Anal Chem 85:325–333

    Article  CAS  Google Scholar 

  9. Torres CM, Pico Y, Manes J (1995) Chromatographia 41:685–692

    CAS  Google Scholar 

  10. Valverde Garcia A, Fernandez Alba AR, Contreras M, Aguera A (1996) J Agric Food Chem 44:1780–1784

    Article  CAS  Google Scholar 

  11. Ueno E, Oshima H, Saito I, Matsumoto H (2001) J Food Hyg Soc Jap 42:385–393

    Article  CAS  Google Scholar 

  12. Fenoll J, Hellin P, Martinez CM, Miguel M, Flores P (2007a) Food Chem 105:711–719

    Article  CAS  Google Scholar 

  13. Fenoll J, Hellin P, Martinez CM, Flores P (2007b) J AOAC Int 90:263–270

    CAS  Google Scholar 

  14. Gelsomino A, Petrovicova B, Tiburtini S, Magnani E, Felici M (1997) J Chromatogr A 782:105–122

    Article  CAS  Google Scholar 

  15. Ueno E, Oshima H, Saito I, Matsumoto H, Nakazawa H (2004) J Food Hyg Soc Jap 45:212–217

    Article  CAS  Google Scholar 

  16. Lehotay SJ, de Kok A, Hiemstra M, van Bodegraven P (2005) J AOAC Int 88:595–614

    CAS  Google Scholar 

  17. Gamón M, Lleó C, Ten A, Mocholí F (2001) J AOAC Int 84:1209–1216

    Google Scholar 

  18. Anastassiades M, Lehotay SJ, Stajnbaher D, Schenck FJ (2003) J AOAC Int 86:412–431

    CAS  Google Scholar 

  19. Lagana A, D’Ascenzo G, Fago G, Marino A (1997) Chromatographia 46:256–264

    Article  CAS  Google Scholar 

  20. Fillion J, Hindle R, Lacroix M, Selwyn J (1995) J AOAC Int 78:1252–1266

    CAS  Google Scholar 

  21. Picó Y, Font G, Moltó JC, Mañes J (2000) J Chromatogr A 882:153–173

    Article  Google Scholar 

  22. Pous X, Font G, Picó Y (2001) Fres J Anal Chem 371:182–189

    Article  CAS  Google Scholar 

  23. Mol HGJ, van Dam RCJ, Steijger OM (2003) J Chromatogr A 1015:119–127

    Article  CAS  Google Scholar 

  24. Paya P, Anastassiades M, Mack D, Sigalova I, Tasdelen B, Oliva J, Barba A (2007) Anal Bioanal Chem 389:1697–1714

    Article  CAS  Google Scholar 

  25. Frenich AG, Vidal JLM, Lopez TL, Aguado SC, Salvador IM (2004) J Chromatogr A 1048:199–206

    Article  Google Scholar 

  26. Cook J, Beckett MP, Reliford B, Hammock W, Engel M (1999) J AOAC Int 82:1419–1435

    CAS  Google Scholar 

  27. Kmellár B, Fodor P, Pareja L, Ferrer C, Martínez-Uroz MA, Valverde A, Fernandez-Alba AR (2008) J Chromatogr A 1215:37–50

    Article  Google Scholar 

  28. Torres CM, Pico Y, Manes J (1996) J Chromatogr A 754:301–331

    Article  CAS  Google Scholar 

Download references

Acknowledgment

The authors are grateful for the financial support of FEDER and European Social Funds, the Ministerio de España de Ciencia e Innovación through the Ramón and Cajal Subprogram.

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Correspondence to José Fenoll.

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Fenoll, J., Hellín, P., Martínez, C.M. et al. Multiresidue Analysis of Pesticides in Vegetables and Citrus Fruits by LC–MS–MS. Chroma 72, 857–866 (2010). https://doi.org/10.1365/s10337-010-1758-8

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  • DOI: https://doi.org/10.1365/s10337-010-1758-8

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