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Feasibility Study for the Production of Certified Calibrants for the Determination of Deoxynivalenol and Other B-Trichothecenes: Intercomparison Study

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Thirteen European laboratories experienced in the analysis of mycotoxins participated in an intercomparison study within a European Commission-funded project. Goals of the study were to check the fitness for purpose of a small batch of gravimetrically prepared calibrants; to compare individually prepared calibrants with common calibrants; to check the feasibility of toxin mixtures as calibrant solutions; and to give recommendations on the production of future certified reference materials (CRMs) with regard to the nature of the calibrant and the means of certification. Each laboratory received ampules of each common calibrant containing single toxins [solution containing either deoxynivalenol (DON), 3-acetyl-DON (3-Ac-DON), nivalenol (NIV), or 15-acetyl-DON (15-Ac-DON)] and 3 ampules of toxinmixture (solutions of DON 3-Ac-DON NIV in acetonitrile) of known concentrations (about 20 g/mL). Ampules with single toxins (solution containing either DON, 3-Ac-DON, NIV, or 15-Ac-DON) and a toxinmixture (solutions of DON 3-Ac-DON NIV in acetonitrile) of unknown concentrations were distributed to the participants for quantification. The participating laboratories used mainly high-performance liquid chromatography (HPLC)diode array detection UV for DON, 3-Ac-DON, NIV, and 15-Ac-DON; gas chromatography-electron capture detection (GC-ECD) and GC-mass spectrometry methods were used sparingly. Linear calibration curves were achieved by >90% of the participants. Relative between-day variation (RSDr) of 26% of the laboratories was greater than the target value of 5% for HPLC, and RSDr of 32% of the laboratories was greater than the desired value of 10% for GC. Relative between-laboratory variation (RSDR) of the GC results obtained with single common calibrants was greater than the target value of 16% for all laboratories. RSDR of the HPLC results for the common unknown single toxin solutions was less than the target value of 8% except for 15-Ac-DON. Generally, better recoveries were observed from common calibrants (102% for mix calibrants and 98% for single calibrants) than from individually prepared calibrants (95%). This international comparison study clearly showed the high scattering of results in the analysis of type-B trichothecenes, particularly when GC was used. Obviously, this intercomparison study was not suited for the certification of B-trichothecenes. A certification of the proposed calibrant material was therefore recommended on the basis of its gravimetrical preparation.

Document Type: Research Article

Affiliations: 1: University of Natural Resources and Applied Life Sciences, Center for Analytical Chemistry, Department for Agrobiotechnology, IFA-Tulln, Vienna, Konrad Lorenz Strasse 20, A-3430 Tulln, Austria. 2: European Commission, DG Joint Research Centre, Institute for Reference Materials and Measurements (JRC-IRMM), Retieseweg, B-2440 Geel, Belgium. 3: National Institute for Public Health and the Environment (RIVM), Laboratory for Food and Residue Analyses (ARO), PO Box 1, 3720 BY Bilthoven, The Netherlands. 4: Swedish University of Agricultural Sciences, Department of Animal Nutrition and Management (SLU), PO Box 7024, S-750 07 Uppsala, Sweden. 5: Central Science Laboratory (CSL), Sand Hutton, York, YO41 1LZ, United Kingdom.

Publication date: 2006-11-01

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  • The Journal of AOAC INTERNATIONAL publishes refereed papers and reviews in the fields of chemical, biological and toxicological analytical chemistry for the purpose of showcasing the most precise, accurate and sensitive methods for analysis of foods, food additives, supplements and contaminants, cosmetics, drugs, toxins, hazardous substances, pesticides, feeds, fertilizers and the environment available at that point in time. The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better methods of preparing samples for analysis; collaborative studies substantiating the performance of a given method; statistical techniques for evaluating data. The Journal will also publish other articles of general interest to its audience, e.g., technical communications; cautionary notes; comments on techniques, apparatus, and reagents.
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