Abstract
We developed a sample preparation method for the determination of polybrominated diphenyl ethers (PBDEs) with from one to ten bromine atoms in samples of feed and food products containing approximately 0.5 g of animal fat or vegetable oil. The method involves gas chromatography with high-resolution mass spectrometry or tandem mass spectrometry. A possibility of using various reagents for the purification of extracts by chemical reactions and fractionation is studied. The physicochemical properties of PBDEs and polychlorinated biphenyls (PCBs) have significant differences, and to determine the full range of PBDEs, it is necessary to use other methods of sample preparation than in the case of PCBs. The conditions selected for the purification of extracts in a column filled with potassium silicate, Florisil, and silica impregnated with sulfuric acid and for their fractionation using activated neutral alumina ensure the PBDE recoveries of at least 75%. Purification of the extracts can be carried out without the use of chlorinated organic solvents. Applied aspects of instrumental analysis and measurement quality assurance are also described.
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
REFERENCES
La Guardia, M.J., Hale, R.C., and Harvey, E., Environ. Sci. Technol., 2006, vol. 40, no. 20, p. 6247.
U.S. Department of Health and Human Services, Toxicological Profile for Polybrominated Biphenyls and Polybrominated Diphenyl Ethers, Atlanta: Public Health Service Aagency for Toxic Substances and Disease Registry, 2004.
Ballschmiter, K. and Zell, M., Fresenius’ Z. Anal. Chem., 1980, vol. 302, p. 20.
Boer, J. and Cofino, W.P., Chemosphere, 2002, vol. 46, no. 5, p. 625.
Berton, P., Lana, N.B., Ríos, J.M., García-Reyes, J.F., and Altamirano, J.C., Anal. Chim. Acta, 2016, vol. 905, p. 24.
Lacorte, S. and Ikonomou, M.G., Chemosphere, 2009, vol. 74, p. 412.
Shin, J., Boo, H., Bang, E., Gorinstein, S., and Seo, J., Eur. Food Res. Technol., 2012, vol. 235, p. 295.
Huwe, J.K., Lorentzsen, M., Thuresson, K., and Bergman, A., Chemosphere, 2002, vol. 46, no. 5, p. 635.
Blanco, S.L. and Vieites, J.M., Anal. Chim. Acta, 2010, vol. 672, nos. 1–2, p. 137.
Pirard, C., De Pauw, E., and Focant, J.-F., J. Chromatogr. A, 2003, vol. 998, nos. 1–2, p. 169.
Wyrzykowska, B., Tabor, D., and Gullett, B.K., Anal. Chem., 2009, vol. 81, no. 11, p. 4334.
Method E3481: The Determination of Polychlorinated Dibenzo-p-Dioxins, Polychlorinated Dibenzofurans, Dioxinlike Polychlorinated Biphenyls (dlPCBs), Polychlorinated Napthalenes (PCNs) and Polybrominated Diphenyl Ethers (PBDEs) in Biota Samples by Automated Sample Extraction/Cleanup and Gas Chromatography–High Resolution Mass Spectrometry (GC–HRMS), Ontario Ministry of the Environment and Climate Change, 2014.
Method 1614: Brominated Diphenyl Ether Congeners in Water, Soil, Sediment, Biosolids and Tissue by HRGC/HRMS, Washington, D.C.: Office of Water Office of Science and Technology Engineering and Analysis Division, 2010.
Method 1668B: Chlorinated Biphenyl Congeners in Water, Soil, Sediment, Biosolids, and Tissue by HRGC/HRMS, Washington, D.C.: Office of Water Office of Science and Technology Engineering and Analysis Division, 2008.
Korytar, P., Covaci, A., Boer, J., Gelbin, A., and Brinkman, U.A.Th., J. Chromatogr. A, 2005, vol. 1065, no. 2, p. 239.
Wei, H., Yang, R., Li, A., Christensen, E.R., and Rockn, K.J., J. Chromatogr. A, 2010, vol. 1217, no. 17, p. 2964.
Eguchi, A., Isobe, T., Ramu, K., Tue, N.M., Sudaryanto, A., Devanathan, G., Viet, P.H., Tana, R.S., Takahashi, S., Subramanian, A., and Tanabe, S., Chemosphere, 2013, vol. 90, no. 3, p. 2365.
Cal, A., Eljarrat, E., and Barcelo, D., J. Chromatogr. A, 2003, vol. 1021, nos. 1–2, p. 165.
Lacorte, S. and Guillamon, M., Chemosphere, 2008, vol. 73, p. 70.
Commission recommendation of 3 March 2014 on the monitoring of traces of brominated flame retardants in food, Official J. Eur. Union, 2014, L 65/39.
Method 1613: Tetra-Through Octa-Chlorinated Dioxins and Furans by Isotope Dilution HRGC/HRMS, Washington, D.C.: Office of Water Engineering and Analysis Division, 1994.
Commission regulation (EU) no. 589/2014 of 2 June 2014 Laying Down Methods of Sampling and Analysis for the Control of Levels of Dioxins, Dioxin-Like PCBs and Non-Dioxin-Like PCBs in Certain Foodstuffs and Repealing Regulation (EU) no. 252/2012, Official J. Eur. Union, 2014, L 164/18.
Wiberg, K., Sporring, S., Haglund, P., and Bjorklund, E., J. Chromatogr. A, 2008, vol. 1138, nos. 1–2, p. 55.
Method 3620c: Florisil Cleanup, 1999.
Shelepchikov, A.A., Brodskii, E.S., Zhil’nikov, V.G., and Feshin, D.B., Mass-Spektrom., 2008, vol. 5, no. 4, p. 245.
Berg, M., Birnbaum, L.S., Denison, M., De Vito, M., Farland, W., Feeley, M., Fiedler, H., Hakansson, H., Hanberg, A., Haws, L., Rose, M., Safe, S., Schrenk, D., Tohyama, C., Tritscher, A., Tuomisto, J., Tysklind, M., Walker, N., and Peterson, R.E., Toxicol. Sci., 2006, vol. 93, no. 2, p. 223.
Fernández-González, V., Grueiro-Noche, G., Concha-Graña, E., Turnes-Carou, M.I., Muniategui-Lorenzo, S., López-Mahía, P., and Prada-Rodríguez, D., Anal. Bioanal. Chem., 2006, vol. 383, no. 2, p. 174.
Raccanelli, S., Guerzoni, S., Rossini, P., and Favotto, M., Organohalogen Compd., 2002, vol. 58, p. 49.
Ferrario, J., Byrne, C., and Dupuy, A.E., Chemosphere, 1997, vol. 34, no. 11, p. 2451.
ACKNOWLEDGMENTS
The authors are grateful to the Center for Ecosystem Safety at the Department of Biology of the Moscow State University for technical support.
Author information
Authors and Affiliations
Corresponding author
Additional information
Translated by O. Zhukova
Rights and permissions
About this article
Cite this article
Shelepchikov, A.A., Ovcharenko, V.V., Kozhushkevich, A.I. et al. A New Method for Purifying Fat-Containing Extracts in the Determination of Polybrominated Diphenyl Ethers. J Anal Chem 74, 574–583 (2019). https://doi.org/10.1134/S1061934819040130
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1134/S1061934819040130