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Reference Material for the Determination of Polychlorodibenzo-p-dioxins, Polychlorodibenzo-furans, and Polychlorinated Biphenyls in Fish: Production Process, Homogeneity, and Stability


Reference Material for the Determination of Polychlorodibenzo-p-dioxins, Polychlorodibenzo-furans, and Polychlorinated Biphenyls in Fish: Production Process, Homogeneity, and Stability



Food Analytical Methods 11(3): 808-823



ISSN/ISBN: 1936-9751

DOI: 10.1007/s12161-017-1062-4

The presence of dibenzo-p-dioxins, polychlorinated dibenzofurans, and polychlorinated biphenyls in food is an important consideration for food safety, especially in fish matrices that are susceptible to bioaccumulation of those compounds from marine environments. In this context, the production of a reference material (RM) for this analytical scope is of great importance for ensuring the reliability of the results generated by monitoring programs. A lyophilized material was produced by spiking tilapia fillets with 29 compounds, and the material was evaluated based on the potential for using it as a certified reference material (CRM) or in proficiency testing (PT) schemes. A pilot experiment was performed to evaluate the incorporation of the analytes in tilapia fillets using standards prepared in nonane and in fish oil. The process yield was approximately 16% for both conditions, but higher mean recoveries were achieved with fish oil. The tilapia fillets were processed, and a portion of this bulk was spiked and then homogenized. The spiked and unspiked portions were frozen prior to lyophilization. Each freeze-dried portion was homogenized and sieved, and then, the portions were mixed, packed, and stored under refrigeration. The material was considered homogeneous for all analytes based on the criteria established for PT. Of the tested analytes, 27 were found to be stable in the short-term design (p > 0.05) when the material was kept at 45 +/- 2 degrees C for 9 days. Long-term stability was evaluated at 2, 4, 6, and 8 months, and 22 of the analytes were found to be stable through up to 4 months of storage based on the criteria defined in references related to both the production of CRM and PT. The contributions of the homogeneity and stability in the short- and long-term uncertainties were estimated and indicated the adequacy of the material for use as a reference for trueness experiments.

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Accession: 070841453

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