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Interlaboratory Comparison of Methods for the Determination of Incurred Tilmicosin Residues in Bovine Liver

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The objective of this study was to compare 2 methods for the determination of tilmicosin residues in bovine liver samples. Three laboratories participated in the comparison of the 2 methods. The first method was described in a New Animal Drug Application (NADA 140–929), and the second was a modification of that method in which hexane was substituted for carbon tetrachloride in one cleanup step. Each of the 3 laboratories analyzed subsamples of 10 bovine livers containing incurred tilmicosin. Residues ranged from 2.3 to 81 ppm tilmicosin in the 10 liver samples with an 11.8% relative standard deviation obtained by using both methods. In addition, fortified-control liver tissue samples were analyzed concurrently with tissues containing incurred residues by using the modified method in one of the laboratories. The fortification levels ranged from 0.3 to 112 ppm, with recoveries ranging from 76 to 92%. The results from the 3 laboratories were comparable, indicating that the modified method was not only as effective as the original NADA method, but also more desirable because of the change to a less hazardous solvent.
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Document Type: Research Article

Affiliations: 1: U.S. Food and Drug Administration, PO Box 25087, Denver, CO 80225. 2: U.S. Food and Drug Administration, Center for Veterinary Medicine, 7500 Standish Pl, Rockville, MD 20855. 3: Western Washington University, Chemistry Department, 516 High St, MS 9150, Bellingham, WA 98225. 4: Colorado State University, Department of Animal Sciences, Ft Collins, CO 80523. 5: U.S. Department of Agriculture, Food Safety and Inspection Service, 4300 Goodfellow Blvd, St. Louis, MO 63120. 6: Elanco Animal Health, 2001 W Main St, Greenfield, IN 46140.

Publication date: 01 November 2002

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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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