Warianty tytułu
Języki publikacji
Abstrakty
A method for simultaneous determination of residues of six organophosphorus pesticides in animal liver samples has been developed and validated. The method is based on the extraction of organophosphorus pesticides with a mixture of acetone-petroleum ether, clean up on a gel permeation chromatography, further clean up on a small silica gel column, and finally determination by gas chromatographx with flame photometric detection. The recovery, investigated by analysing blank liver samples spiked with chlorpyrifos-methyl, chlorpyrifos, diazinon, parathion, and pirimiphos-methyl at levels of 5, 25, 50, and 75 µg/kg, and with chlorfenvinphos at levels of 5, 10, and 15 µg/kg, ranged from 75.6% to 107.5%. Performance characteristics, such as repeatability and within-laboratory reproducibility, expressed as coefficient of variation, were less than 20%, and uncertainty <21%. Linearity ranged between 5 and 1,000 ng/mL. The limits of quantification were 5 µg/kg for all compounds and allowed determination of residues below the MRLs set by the European Union. The satisfacton z-score results of international proficiency tests confirmed good accuracy, reproducibility, and reliability of the developed method.
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Opis fizyczny
p.731-736,fig.,ref.
Twórcy
autor
- Department of Pharmacology and Toxicology, National Veterinary Research Institute, 24-100 Pulawy, Poland
autor
autor
Bibliografia
- 1. Bennett D.A., Chung A.C., Lee S.M.: Multiresidue method for analysis of pesticides in liquid whole milk. J AOAC Int 1997, 80, 1065-1077.
- 2. Chung S.W., Chan B.T.: Validation and use of a fast sample preparation method and a liquid chromatography-tandem mass spectrometry in analysis of ultra-trace levels of 98 organophosphorus pesticide and carbamate residues in total diet study involving diversified food types. J Chromatogr A 2010, 1217, 4815-4824.
- 3. Di Muccio A., Pelosi P., Camoni I., Attard Barbini D., Dommarco R., Generali T., Ausili A.: Selective, solid-matrix dispersion extraction of organophosphate pesticide residues from milk. J Chromatogr A 1996, 754, 497-506.
- 4. EN 1528 Fatty food - Determination of pesticides and polychlorinated biphenyls (PCBs)-part 1-4, 1996.
- 5. Eurachem/CITAC Guide. Quantifying uncertainty in analytical measurement. Second edition. 2000.
- 6. Garcia de Llasera M.P., Reyes-Reyes M.L.: A validated matrix solid-phase dispersion method for the extraction of organophosphorus pesticides from bovine samples. Food Chemistry 2009, 114, 1510-1516.
- 7. Garrido Frenich A., Martinez Vidal J.L., Cruz Sicilia A.D., Gonzalez Rodriguez M.J., Plaza Bolaños P.: Multiresidue analysis of organochlorine and organophosphorus pesticides in muscle of chicken, pork and lamb by gas chromatography-triple quadrupole mass spectrometry. Anal Chim Acta 2006, 558, 42-52.
- 8. Garrido Frenich A., Plaza Bolaños P., Martinez Vidal J.L.: Multiresidue analysis of pesticides in animal liver by gas chromatography using triple quadrupole tandem mass spectrometry. J Chromatogr A 2007, 1153, 194-202.
- 9. Juhler R.K: Optimized method for the determination of organophosphorus pesticides in meat and fatty matrices. J Chromatogr A 1997, 786, 145-153.
- 10. Juhler R.K: Supercritical fluid extraction of pesticides from meat: a systematic approach for optimisation. Analyst 1998, 123, 1551-1556.
- 11. Navas Diaz A., Garcia Pareja A., Garcia Sanchez F.: Liquid and gas chromatographic multi-residue pesticide determination in animal tissues. Pestic Sci 1997, 49, 56-64.
- 12. Pagliuca G., Gazzotti T., Zironi E., Sticca P.: Residue analysis of organophosphorus pesticides in animal matrices by dual column capillary gas chromatography with nitrogen-phosphorus detection. J Chromatogr A 2005, 1071, 67-70.
- 13. Pang G.F., Cao Y.Z., Fan C.L., Jia G.Q., Zhang J.J., Li X.M., Liu Y.M., Shi Y.Q., Li Z.Y., Zheng F., Lian Y.J.: Analysis method study on 839 pesticide and chemical contaminant multiresidues in animal muscles by gel permeation chromatography cleanup, GC/MS, and LC/MS/MS. J AOAC Int 2009, 92, 1-72.
- 14. Regulation (EC) No. 396/2005 of the European Parliament and of the Council of 23 February 2005 on maximum residue levels of pesticides in or on food and feed of plant and animal origin and amending Council Directive 91/414/EEC. OJ L 2005, 70.
- 15. Rimkus G.G., Rummler M., Nausch I.: Gel permeation chromatography-high-performance liquid chromatography combination as an automated clean-up technique for the multiresidue analysis of fats. J Chromatogr A 1996, 737, 9-14.
- 16. Rosenblum L., Hieber T., Morgan J.: Determination of pesticides in composite dietary samples by gas chromatography/mass spectrometry in the selected ion monitoring mode by using a temperature-programmable large volume injector with preseparation column. J AOAC Int 2001,84, 891 -900.
- 17. Salas J.H., González M.M., Noa M., Pérez N.A, Díaz G., Gutiérrez R., Zazueta H., Osuna I.: Organophosphorus pesticide residues in Mexican commercial pasteurized milk. J Agric Food Chem 2003, 51, 4468-4471.
- 18. SANCO/10684/2009. Method validation and qualitx control procedures for pesticide residues analysis in food and feed.
- 19. Sannino A., Mambriani P., Bandini M., Bolzoni L.: Multiresidue method for determination of organophosphorus insecticide residues in fatty processed foods by gel permeation chromatography. J AOAC Int 1995, 78, 1502-1512.
- 20. Schenck F.J., Donoghue D.J.: Determination of organochlorine and organophosphorus pesticide residues in eggs using a solid phase extraction cleanup. J Agric Food Chem 2000, 48, 6412-6415.
- 21. Schenck F.J., Wagner R.: Screening procedure for organochlorine and organophosphorus pesticide residues in milk using matrix solid phase dispersion (MSPD) extraction and gas chromatographic determination. Food Addit Contam Part A 1995, 12, 535-541.
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Bibliografia
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