González de la Huebra María José, Vincent Ursula, Serano Federica, von Holst Christoph
European Commission, Joint Research Centre, Institute for Reference Materials and Measurements (EC-JRC-IRMM), Retieseweg 111, B-2440 Geel, Belgium.
J AOAC Int. 2012 Jan-Feb;95(1):61-6. doi: 10.5740/jaoacint.10-499.
The performance characteristics of a method based on HPLC with postcolumn derivatization and spectrophotometric detection for the quantification of semduramicin in poultry feedingstuffs have been determined via a collaborative study. Semduramicin is a feed additive that is authorized for fattening chickens within the European Union at a minimum and maximum content of 20 and 25 mg/kg in feedingstuffs, respectively. The target concentration of semduramicin in the test samples ranged from 11.5 to 45.0 mg/kg. The study has been conducted with two different types of test material, namely, feedingstuff samples that have been previously ground in our laboratory and pelleted feedingstuffs. In the latter case, the laboratories participating in the study had to grind the samples prior to analysis. The obtained RSD for repeatability (RSD(r)) ranged from 2 to 10% for the ground materials, and from 2 and 7% for the pelleted materials. The RSD for reproducibility (RSDR) varied between 11 and 16% for the ground materials, and between 12 and 15% for the pelleted materials. These data indicated that grinding as an additional step in the analytical procedure did not influence the precision profile of the method. In addition, the HorRat values for all test materials were below or equal to 1.5, thus demonstrating that the obtained precision data were acceptable for the purpose of the method. Furthermore, an estimation of trueness based on statistical treatment of the results reported from the laboratories for spiked samples revealed acceptable mean recovery values of 88 +/- 4%. Based on the obtained performance profile, the method can be considered fully validated and transferable to control laboratories to be used within the framework of official control.
通过一项协同研究，已确定了一种基于高效液相色谱法（HPLC）并采用柱后衍生化和分光光度检测法对家禽饲料中塞杜霉素进行定量分析的方法的性能特征。塞杜霉素是一种饲料添加剂，在欧盟被批准用于育肥鸡，饲料中的最低和最高含量分别为20毫克/千克和25毫克/千克。测试样品中塞杜霉素的目标浓度范围为11.5至45.0毫克/千克。该研究使用了两种不同类型的测试材料，即先前在我们实验室研磨过的饲料样品和颗粒饲料。在后一种情况下，参与研究的实验室在分析前必须将样品研磨。对于研磨后的材料，重复性相对标准偏差（RSD(r)）范围为2%至10%，对于颗粒材料，范围为2%至7%。再现性相对标准偏差（RSDR）对于研磨后的材料在11%至16%之间，对于颗粒材料在12%至15%之间。这些数据表明，研磨作为分析程序中的一个额外步骤不会影响该方法的精密度。此外，所有测试材料的HorRat值均低于或等于1.5，因此表明所获得的精密度数据对于该方法的目的而言是可接受的。此外，基于对实验室报告的加标样品结果进行统计处理的准确性估计显示，平均回收率值为88±4%，可接受。基于所获得的性能概况，该方法可被认为已得到充分验证，并且可转移至控制实验室，以便在官方控制框架内使用。
