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

• Autorzy: Boneva Iskra , Yaneva Spaska , Danalev Dancho

Identyfikatory

DOI

10.1556/1326.2020.00778

• Języki publikacji: EN

Abstrakty

EN

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.

Słowa kluczowe

EN

organophosphorus pesticides; GC-MS/MS ion-trap; food analysis; liver samples

• Wydawca: University of Silesia in Katowice ; Akademiai Kiado
• Czasopismo: Acta Chromatographica
• Rocznik: 2021
• Tom: Vol. 33, no. 2
• Strony: 188--194
• Opis fizyczny: Bibliogr. 24 poz., rys., tab.

Twórcy

autor

Boneva Iskra

• Central Laboratory of Veterinary Control and Ecology (CLVCE), Bulgarian Food Safety Agency, 5 Iskarsko Shousse Str, Sofia, Bulgaria

autor

Yaneva Spaska

• University of Chemical Technology and Metallurgy, 8 blvd. Kliment Ohridski, Sofia, 1756, Bulgaria

autor

Danalev Dancho

• University of Chemical Technology and Metallurgy, 8 blvd. Kliment Ohridski, Sofia, 1756, Bulgaria

• https://orcid.org/0000-0003-1193-7379

Bibliografia

• 1. Whitford, F. The Benefits of Pesticides, A Story Worth Telling. Purdue Extension, https://www.extension.purdue.edu/extmedia/ppp/ppp-70.pdf, 2009. Retrieved March 27, 2020.
• 2. Gilden, R. C.; Huffling, K.; Sattler, B. Pesticides and health risks. J. Obstet. Gynecol. Neonatal Nurs. 2010, 39, 103. https://doi.org/10.1111/j.1552-6909.2009.01092.x.
• 3. Kiljanek, T.; Niewiadowska, A.; Semeniuk, S. Determination of organophosphorus pesticide residues in the liver by gas chromatography with flame photometric detection. Bull. Vet. Inst. Pulawy 2011, 55 731.
• 4. Colović, M. B.; Krstić, D. Z.; Lazarević-Pašti, T. D.; Bondžić, A. M.; Vasić, V. M. Acetylcholinesterase inhibitors: pharmacology and toxicology. Curr. Neuropharmac. 2013, 11, 315. https://doi.org/10.2174/1570159X11311030006.
• 5. Commission Implementing Regulation (EU) 2018/555 of 9 April 2018 Concerning a Coordinated Multiannual Control Programme of the Union for 2019, 2020 and 2021 to Ensure Compliance with Maximum Residue Levels of Pesticides and to Assess the Consumer Exposure to Pesticide Residues in and on Food of Plant and Animal Origin, https://eur-lex.europa.eu/eli/reg_impl/2018/555/oj. Retrieved March 27, 2020.
• 6. Stoykova, T.; Yankovska-Stefenova, T.; Yotova, L. Danalev, D. Modified QuECHERS method for determination of methomyl, aldicarb, carbofuran and propoxur in liver. Shemistry: Bulg. J. Sci. Educ. 2015, 24, 390.
• 7. Yaneva, S.; Stoykova, I.; Danalev, D.; Yotova, L. Determination of N-methyl carbamates in a liver sample using an optical biosensor. JCTM 2019, 54, 362.
• 8. Ledoux, M. Analytical methods applied to the determination of pesticide residues in foods of animal origin. A review of the past two decades. J. Chromatogr. A 2011, 1218, 1021.
• 9. Anastassiades, M.; Lehotay, S. J.; Stajnbaher, D.; Schenck, F. J. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce. J. AOAC Int. 2003, 86, 412.
• 10. Aguilera-Luiz, M. M.; Vidal, J. L. M.; Romero-González, R.; Frenich, A. G. Multi-residue determination of veterinary drugs in milk by ultra-high pressure liquid chromatograph- tandem mass spectrometry. J. Chromatogr. A 2008, 1205, 10.
• 11. Cunha, S. C.; Lehotay, S. J.; Mastovska, K.; Fernandes, J. O.; Beatriz, M.; Oliveira, P. P. Evaluation of the QuEChERS sample preparation approach for the analysis of pesticide residues in olives. J. Sep. Sci.2007, 30, 620.
• 12. Lehotay, S. J.; Mastvoska, K.; Yun, S. J. Evaluation of two fast and easy methods for pesticide residue analysis in fatty food matrixes. J. AOAC Int. 2005, 88, 630.
• 13. Lehotay, S. J.; Son, K. A.; Kwon, H.; Koesukwiwat, U.; Fu, W.; Mastovska, K.; Hoh, E.; Leepipatpiboon, N. Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables. J. Chromatogr. A 2010, 1217, 2548.
• 14. Beyer, A.; Biziuk, M. Applications of sample preparation techniques in the analysis of pesticides and PCBs in food. Food Chemistry 2008, 108, 669.
• 15. Beyer, A.; Biziuk, M. Analytical methods for the routinely evaluation of pesticide residues in lemon fruits and by products. SN App. Sci. 2019, 1, 618.
• 16. BDS EN 1528–1:2001 Fatty food – Determination of pesticides and polychlorinated biphenyls (PCBs). Part 1: General, Bulgarian Institute for Standardization.
• 17. Przybylski, C.; Segard, C. Method for routine screening of pesticides and metabolites in meat based baby-food using extraction and gas chromatography-mass spectrometry, J. Sep. Sci. 2009, 32, 1858.
• 18. Castillo, M.; Carbonell, E.; Gonzàlez, C.; Miralles-Marco, A. Pesticide Residue Analysis in Animal Origin Food: Procedure Proposal and Evaluation for Lipophilic Pesticides, Open Access Book “Pesticides – Resent Trends in Pesticides Residues Assay”, ISBN 978-953-51-0681-4, Chapter 3; Publisher InTech, 2012.
• 19. Main changes introduced in Document Nº SANTE/12682/2019 with respect to the previous version (Document Nº SANTE/11813/2017). Guidance document on analytical quality controland validation procedures for pesticide residues analysis in food and feed.
• 20. EURACHEM/CITAC Guide CG 4, Quantifying Uncertainty in Analytical Measurement, Ellison, S. L. R.; Williams A. Eds, 3rd ed., https://www.eurachem.org/images/stories/Guides/pdf/QUAM2012_P1.pdf. Retrieved March 27, 2020.
• 21. Kiljanek, T.; Niewiadowska, A.; Semeniuk, S. Determination of organophosphorus pesticide residues in the liver by gas chromatography with flame photometric detection. Bull. Vet. Inst. Pulawy 2011, 55, 731.
• 22. Botitsi, H. V.; Garbis, S. D.; Economou, A.; Tsipi, D. F. Current mass spectrometry strategies for the analysis of pesticides and their metabolites in food and water matrices. Mass Spectrom. Rev. 2011, 30, 907.
• 23. Chung, S. W. C.; Chen, B. L. S. Determination of organochlorine pesticide residues in fatty foods: A critical review on the analytical methods and their testing capabilities. J. Chromatogr. A 2011, 1218, 5555.
• 24. Zanella, R.; Prestes, O. D.; Do Amaral, F. C.; Martins, M. L.; Bohrer, A. M. Modern Sample Preparation Methods for Pesticide Multiresidue Determination in Foods of Animal Origin by Chromatographic-mass Spectrometric Techniques. Open access Book: The impact of pesticides. AcademyPublish.org, 2012, ISBN 978-0- 9835850-9-1, 355–379.

Uwagi

Opracowanie rekordu ze środków MNiSW, umowa Nr 461252 w ramach programu "Społeczna odpowiedzialność nauki" - moduł: Popularyzacja nauki i promocja sportu (2021).