Analytical and Bioanalytical Chemistry

, Volume 411, Issue 27, pp 7281–7291 | Cite as

LC-MS/MS method for the determination of organophosphorus pesticides and their metabolites in salmon and zebrafish fed with plant-based feed ingredients

  • Borja Garlito
  • María Ibáñez
  • Tania Portolés
  • Roque Serrano
  • Heidi Amlund
  • Anne-Katrine Lundebye
  • Monica Sanden
  • Marc H. G. BerntssenEmail author
  • Félix HernándezEmail author
Research Paper


The composition of Atlantic salmon feed has changed considerably over the last two decades from being marine-based (fishmeal and fish oil) to mainly containing plant ingredients. Consequently, concern related to traditional persistent contaminants typically associated with fish-based feed has been replaced by other potential contaminants not previously associated with salmon farming. This is the case for many pesticides, which are used worldwide to increase food production, and may be present in plant ingredients. Earlier studies have identified two organophosphorus pesticides, chlorpyrifos-methyl and pirimiphos-methyl, in plant ingredients used for aquafeed production. In the present study, we developed a reliable and sensitive analytical method, based on liquid chromatography coupled to tandem mass spectrometry, for the determination of these pesticides and their main metabolites in warm water (zebrafish) and cold water (Atlantic salmon) species, where possible differences in metabolites could be expected. The method was tested in whole zebrafish and in different salmon tissues, such as muscle, bile, kidney, fat, and liver. The final objective of this work was to assess kinetics of chlorpyrifos-methyl and pirimiphos-methyl and their main metabolites in fish tissue, in order to fill the knowledge gaps on these metabolites in fish tissues when fed over prolonged time.


Chlorpyrifos-methyl Pirimiphos-methyl Metabolites Atlantic salmon Zebrafish LC-MS/MS 



The authors wish to thank the staff at the Skretting ARC, Lerang Research Station for their excellent help with sampling and conducting the feeding trial. Tania Portolés acknowledges Ramon y Cajal Program from the Ministry of Economy and Competitiveness (RYC-2017-22525) for funding her research.

Funding information

The present work was financed by the Norwegian Research Council (NFR) project “AQUASAFE” (254807).

Compliance with ethical standards

Conflict of interest

The authors declare that there is no conflict of interest.

Research involving animals

The experiment complied with the guidelines of the Norwegian Regulation on Animal Experimentation and EC Directive 86/609/EEC. The National Animal Research Authority approved the protocol (ID 12091).

Supplementary material

216_2019_2104_MOESM1_ESM.pdf (99 kb)
ESM 1 (PDF 98 kb)


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Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2019

Authors and Affiliations

  • Borja Garlito
    • 1
  • María Ibáñez
    • 1
  • Tania Portolés
    • 1
  • Roque Serrano
    • 1
  • Heidi Amlund
    • 2
  • Anne-Katrine Lundebye
    • 3
  • Monica Sanden
    • 3
  • Marc H. G. Berntssen
    • 3
    Email author
  • Félix Hernández
    • 1
    Email author
  1. 1.Research Institute for Pesticides and Water (IUPA)University Jaume ICastellón de la PlanaSpain
  2. 2.Technical University of Denmark (DTU)Kgs. LyngbyDenmark
  3. 3.National Institute of Nutrition and Seafood ResearchBergenNorway

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