Determination of tiamulin in Type C medicated swine feeds using high throughput extraction with liquid chromatography

An improved method for extraction and analysis of tiamulin is presented to address issues that arose during routine analysis of Type C medicated swine feeds under the current U.S. Food and Drug Administration-Center for Veterinary Medicine (FDA-CVM) approved method. The issues included the need for higher sample throughput and the ability to accommodate a wider variety of feed matrixes. Changes to the FDA-CVM approved method include reduced sample size and solvent volumes, phosphate buffering of tartaric acid, centrifugation, and use of a new liquid chromatography column and adjusted mobile phase composition. A paired sample study was performed to compare performance of the new and existing methods. The paired sample study showed no statistical difference between sample means of paired sets of 17 samples analyzed by both methods (t = 1.95 at 0.05 significance level, p = 0.068). A recovery study showed the method precision to be 2.06% (coefficient of variation) with an average standard recoveryof 95.8%. Ruggedness test results indicated good overall ruggedness of the method.