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      Development and validation of method for determination of organophosphorus pesticides traces in liver sample by GC-MS/MS-ion trap

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          A method for simultaneous determination of trace of four organophosphorus pesticides residues in animal liver samples has been developed and validated. This method is based on the preliminary sample preparation using extraction of target compound with a mixture of toluene-cyclohexane by means of up-to-date accelerated solvent extraction (ASE), liquid-liquid partitioning with acetonitrile and hexane, additional clean up step using QuEChERS method. Further the obtained analytes are determined by gas chromatography with ion-trap detector. The validation of the method is performed in accordance with the recommendations in Document SANTE/11945/2015 and it meets the acceptability criteria for precision, mean recovery and limits of quantification. The samples were investigated by analysing blank liver samples and samples spiked with the target analytes chlorpyrifos-methyl, parathion and pirimiphos-methyl at levels of 25, 50, and 75 ng/g and with diazinon at levels of 15, 30, and 45 ng/g. The recovery for all compounds were in the range from 73 to 104% which perfectly fit with requirements of documents and European legislations. The repeatability and within-laboratory reproducibility also reveal acceptable in documents coefficient of variation and uncertainty less than 20 and 18%, respectively. The limits of quantification were less than 3 ng/g for all compounds and allowed determination of residues below the maximum residue levels (MRLs) set in Regulation (EC) Nº 396/2005.

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          Author and article information

          Acta Chromatographica
          Acta Chromatographica
          Akadémiai Kiadó (Budapest )
          19 March 2021
          17 July 2020
          : 33
          : 2
          : 188-194
          [1 ] Central Laboratory of Veterinary Control and Ecology (CLVCE), Bulgarian Food Safety Agency , 5 Iskarsko Shousse Str, Sofia, Bulgaria
          [2 ] University of Chemical Technology and Metallurgy , 8 blvd. Kliment Ohridski, Sofia, 1756, Bulgaria
          Author notes
          [* ]Corresponding author. Tel.: +359 2 8163310. E-mail: ddanalev@ 123456uctm.edu
          © 2020 The Authors

          Open Access statement. This is an open-access article distributed under the terms of the Creative Commons Attribution-NonCommercial 4.0 International License ( https://creativecommons.org/licenses/by-nc/4.0/), which permits unrestricted use, distribution, and reproduction in any medium for non-commercial purposes, provided the original author and source are credited, a link to the CC License is provided, and changes – if any – are indicated.

          Page count
          Figures: 1, Tables: 4, Equations: 0, References: 24, Pages: 07

          Materials properties,Nanomaterials,Chemistry,Nanotechnology,Analytical chemistry,Thin films & surfaces
          food analysis,GC-MS/MS ion-trap,organophosphorus pesticides,liver samples


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