, Volume 68, Supplement 1, pp 49–55 | Cite as

Fast GC–MS Pesticide Multiresidue Analysis of Apples

  • Renáta Húšková
  • Eva Matisová
  • Michal Kirchner


A fast gas chromatographic–mass spectrometric (GC–MS) method is proposed for pesticide multiresidue analysis of apples. The QuEChERS method was used for sample preparation. GC–MS analysis was performed with a PTV, an autoinjector, and a quadrupole benchtop MS detector. Electron-impact ionization (70 eV) was used with two modes of selected ion monitoring. Compounds were separated under temperature-programmed conditions on a narrow-bore diphenyldimethylsiloxane column. In one chromatographic run 61 pesticides of different chemical classes, and triphenyl phosphate as internal standard, were determined in 11 min. Calibration was performed with matrix-matched standard solutions and response to the pesticides was a linear function of concentration in the range 1–500 ng mL−1 (equivalent to 1–500 μg kg−1 in real samples). High values of the determination coefficients (R 2; 0.9900–1.0000) were obtained for most of the pesticides. Limits of detection and quantification were determined. When the method was used for analysis of pesticide residues in real samples, five pesticides were detected at concentrations in the range 1.00–21.47 μg kg−1. Repeatability of measurements, expressed as relative standard deviations of absolute peak areas, normalized relative to TPP, and of the concentrations determined, met the EU criterion of RSD ≤ 20%. Use of the internal standard moderately improved quantitative results.


Gas chromatography Fast GC–MS Multiresidue analysis Pesticide residues Calibration 



This work was supported by the Slovak Research and Development Agency under contract no. 20-000705 and partially supported within the framework of the Slovak Grand Agency (VEGA, project number 1/2463/05).


  1. 1.
    European Union Introduction to EC pesticides residues legislation, European Union, Brussels;
  2. 2.
    European Union (1999) Commission Directive 1999/39/EC amending Directive 95/5/EC. Off J Eur Com L 124/8Google Scholar
  3. 3.
    Hercegová A, Dömötörová M, Matisová E (2007) J Chromatogr A 1153:54–73CrossRefGoogle Scholar
  4. 4.
    van Deursen MM, Beens J, Janssen HG, Leclerq PA, Cramers CA (2000) J Chromatogr A 878:205–213CrossRefGoogle Scholar
  5. 5.
    Kirchner M, Matisová E, Otrekal R, Hercegová A, de Zeeuw J (2005) J Chromatogr A 1084:63–70CrossRefGoogle Scholar
  6. 6.
    Kirchner M, Matisová E, Hrouzková S, de Zeeuw J (2005) J Chromatogr A 1090:126–132CrossRefGoogle Scholar
  7. 7.
    Hercegová A, Dömötörová M, Matisová E, Kirchner M, Otrekal R, Štefuca V (2005) J Chromatogr A 1084:46–53CrossRefGoogle Scholar
  8. 8.
    Hercegová A, Dömötörová M, Kružlicová D, Matisová E (2006) J Sep Sci 29:1102–1109CrossRefGoogle Scholar
  9. 9.
    Kirchner M, Húšková R, Matisová E, Mocák J (2007) J Chromatogr A (submitted)Google Scholar
  10. 10.
    Hajšlová J, Zrostlíková J (2003) J Chromatogr A 1000:181–197CrossRefGoogle Scholar
  11. 11.
    Korytár P, Janssen HG, Matisová E, Brinkman UATh (2002) Trends Anal Chem 21:558–572CrossRefGoogle Scholar
  12. 12.
    Matisová E, Dömötörová MJ (2003) J Chromatogr A 1000:199–221CrossRefGoogle Scholar
  13. 13.
    Anastassiades M, Lehotay SJ, Štajbaher D, Schenck FJ (2003) JAOAC 86:412–431Google Scholar
  14. 14.
    Godula R, Hajšlová J, Alterová K (1999) J High Resolut Chromatogr 22:395–402CrossRefGoogle Scholar
  15. 15.
    Zrostlíková J, Hajšlová J, Godula M, Maštovská K (2001) J Chromatogr A 937:73–86CrossRefGoogle Scholar
  16. 16.
    Čajka T, Hajšlová J (2004) J Chromatogr A 1058:251–261Google Scholar
  17. 17.
    Dömötörová M, Matisová E, Kirchner M, de Zeeuw J (2005) Acta Chim Slov 52:422–428Google Scholar
  18. 18.
    Leandro CC, Hancock P, Fussell RJ, Kelly BJ (2006) J Chromatogr A 1103:94–101CrossRefGoogle Scholar
  19. 19.
    Anastassiades M, Maštovská K, Lehotay SJ (2003) J Chromatogr A 1015:163–184CrossRefGoogle Scholar
  20. 20.
    Čajka T, Maštovská K, Lehotay SJ, Hajšlová J (2005) J Sep Sci 28:1048–1060CrossRefGoogle Scholar
  21. 21.
    Maštovská K, Lehotay SJ, Anastassiades M (2005) Anal Chem 77:8129–8137CrossRefGoogle Scholar
  22. 22.
    Dalluge J, Vreuls RJJ, van Iperen DJ, van Rijn M, Brinkman UA Th (2002) J Sep Sci 25:608–614CrossRefGoogle Scholar
  23. 23.
    Maštovská K, Lehotay SJ (2003) J Chromatogr A 1000:153–180CrossRefGoogle Scholar
  24. 24.
    Amirav A, Jing H (1995) Anal Chem 67:3305–3318CrossRefGoogle Scholar
  25. 25.
    European Union (1994) Council Directives 94/43/EC. Off J Eur Com L 227 31Google Scholar

Copyright information

© Friedr. Vieweg & Sohn Verlag/GWV Fachverlage GmbH 2008

Authors and Affiliations

  • Renáta Húšková
    • 1
  • Eva Matisová
    • 1
  • Michal Kirchner
    • 1
  1. 1.Institute of Analytical Chemistry, Faculty of Chemical and Food TechnologySlovak University of TechnologyBratislavaSlovak Republic

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