Analysis of 52 pesticides in fresh fish muscle by QuEChERS extraction 1 followed by LC-MS/MS determination

Pesticide pollution in water has been well described; however, little is known on pesticide accumulation by aquatic organisms, and to date, most studies in this line have been focused on persistent organochlorine pesticides. For this reason, a method based on QuEChERS extraction and subsequent liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis has been developed and validated for the determination of 52 medium to highly polar pesticides in fresh fish muscle. Target pesticides were selected on the basis of use and occurrence in surface waters. Quantification is carried out following an isotope dilution approach. The method developed is satisfactory in terms of accuracy (relative recoveries between 71 and 120%), precision (relative standard deviations below 21%) and sensitivity (limits of determination in the pg/g or low ng/g f.w. range for most compounds). The application of the validated methodology to fish specimens collected from the Adige River (Italy) revealed the presence of trace levels of diazinon, dichlorvos and diuron, and measurable levels of metolachlor, quinoxyfen, irgarol, terbutryn, and acetamiprid, but in all cases at concentrations below the default maximum residue level of 10 ng/g established for pesticides not specifically regulated in fish intended for human consumption. Metolachlor and quinoxyfen were both the most ubiquitous and abundant pesticides, in agreement with their high potential for bioaccumulation. Both are toxic to aquatic organisms, and therefore, their potential effects on aquatic ecosystems should be further explored. © 2018 Elsevier B.V.The authors thank the financial support of the EU ( FP7 projects GLOBAQUA ( 265264 ) and SOLUTIONS ( 603437 )) and the Generalitat de Catalunya (Consolidated Research Group “ 2017 SGR 1404 - Water and Soil Quality Unit”). Bekolut is acknowledged for the gift of QuEChERS kits. CP acknowledges support from the Swedish University of Agricultural Sciences through the August T Larsson Guest Researcher Programme. Appendix APeer reviewe