Analytical and Bioanalytical Chemistry

, Volume 409, Issue 26, pp 6181–6193 | Cite as

Determination of pesticides in sewage sludge from an agro-food industry using QuEChERS extraction followed by analysis with liquid chromatography-tandem mass spectrometry

  • Laura Ponce-Robles
  • Gracia Rivas
  • Belen Esteban
  • Isabel Oller
  • Sixto Malato
  • Ana AgüeraEmail author
Research Paper


An analytical method was developed and validated for the determination of ten pesticides in sewage sludge coming from an agro-food industry. The method was based on the application of Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction for solid sewage sludge and SPE extraction for sludge aqueous phase, followed by liquid chromatography (LC) coupled to hybrid quadrupole/linear ion trap mass spectrometry (QqLIT-MS). The QuEChERS method was reported 14 years ago and nowadays is mainly applied to the analysis of pesticides in food. More recent applications have been reported in other matrices as sewage sludge, but the complexity of the matrix makes necessary the optimization of the cleanup step to improve the efficiency of the analysis. With this aim, several dispersive solid-phase extraction cleanup sorbents were tested, choosing C18 + PSA as a d-SPE sorbent. The proposed method was satisfactorily validated for most compounds investigated, showing recoveries higher than 80% in most cases, with the only exception of prochloraz (71%) at low concentration level. Limits of quantification were lower than 40 ng l−1 in the aqueous phase and below 40 ng g−1 in the solid phase for the majority of the analytes. The method was applied to solid sludge and the sludge aqueous phase coming from an agro-food industry which processes fruits and vegetables.

Graphical abstract

Application of LC/MS/MS advanced analytical techniques for determination of pesticides contained in sewage sludge


Agro-food industry Industrial wastewater LC-MS Pesticides Sludge QuEChERS 



The authors wish to thank the Junta de Andalucía (Andalusian Regional Government in Spain) (RNM-1739) and the European Regional Development Fund (ERDF) for funding this investigation.

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.


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Copyright information

© Springer-Verlag GmbH Germany 2017

Authors and Affiliations

  • Laura Ponce-Robles
    • 1
    • 2
  • Gracia Rivas
    • 2
  • Belen Esteban
    • 2
  • Isabel Oller
    • 1
    • 2
  • Sixto Malato
    • 1
    • 2
  • Ana Agüera
    • 2
    Email author
  1. 1.Plataforma Solar de Almería-CIEMATTabernasSpain
  2. 2.CIESOL, Joint Centre of the University of Almería-CIEMATLa Cañada de San UrbanoSpain

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