Moore Douglas B, Britton Nanc L, Smallidge Robert L, Riter Ken L
Purdue University, Office of Indiana State Chemist, West Lafayette 47907, USA.
J AOAC Int. 2002 May-Jun;85(3):533-40.
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.
本文提出了一种改进的替米考星提取与分析方法,以解决在美国食品药品监督管理局兽医中心(FDA - CVM)现行批准方法对C型加药猪饲料进行常规分析时出现的问题。这些问题包括需要更高的样品通量以及能够适应更多种类的饲料基质。对FDA - CVM批准方法的改进包括减小样品量和溶剂量、用磷酸盐缓冲酒石酸、离心,以及使用新的液相色谱柱和调整流动相组成。进行了配对样品研究以比较新方法和现有方法的性能。配对样品研究表明,两种方法分析的17对配对样品的样本均值之间无统计学差异(在0.05显著性水平下,t = 1.95,p = 0.068)。回收率研究表明该方法的精密度为2.06%(变异系数),平均标准回收率为95.8%。耐用性测试结果表明该方法总体耐用性良好。