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Determination of Maduramicin in Feedingstuffs and Premixtures by Liquid Chromatography: Development, Validation, and Interlaboratory Study

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A reversed-phase liquid chromatography method for determination of maduramicin in feedingstuffs and premixtures was developed, validated, and interlaboratory studied. The extraction solvent was methanol. Maduramicin was detected at 520 nm after postcolumn derivatization with vanillin. Recovery was >90%. The repeatability relative standard deviation (RSDr) in feeds (1–5 mg/kg) and premixtures (500 mg/kg) ranged between 2.7 and 7.7%; the within-laboratory reproducibility was between 3.7 and 8.5%. The limit of quantitation was 2 mg/kg. Other feed additives did not interfere in the assay. The method showed ruggedness against small changes in the extraction conditions, eluant composition, and conditions for postcolumn derivatization. The presence of water in the extraction solvent negatively affected the recovery. In the collaborative study, 5 feeds (4 positive at 2.5–9 mg/kg, 1 blank) and 1 premixture (450 mg/kg) were analyzed by 10 laboratories. The RSDr of the feedingstuffs varied between 3.29 and 8.53%. The HORRAT ranged between 1.10 and 1.98. Recoveries were >90%, except for one participant (80%). One laboratory detected small signals in the blank sample, corresponding to 0.7 and 0.8 mg/kg. For the premixture, the RSDr was 3.15% and the HORRAT was 1.80.
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Document Type: Research Article

Affiliations: 1: RIKILT-Institute of Food Safety, PO Box 230, 6700 AE, Wageningen, The Netherlands. 2: Austrian Agency for Health and Food Safety, Agricultural Inspection Service and Research Centre Vienna (AGES-LWVIE), Spargelfeldstraße 191, A-1226 Vienna, Austria. 3: Hoffmann-La Roche Ltd., Bau 71/248, CH-4070, Basel, Switzerland. 4: Universität Hamburg, Institut für Angewandte Botanik, PO Box 302762, D-20309, Hamburg, Germany.

Publication date: 2004-09-01

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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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