Expanded Testing Methods for Elements and Metals in Animal Diagnostic Specimens

1 项目概要： FDA 目前缺乏生前（活体）的标准化方法 2 动物）和动物诊断标本的尸检分析可能与 3 动物食品/饲料污染事件。为了弥补这一差距，现有的 FDA 方法必须 4 扩展到新基质的测试，如牛奶、尿液、血液和组织。目的 5 该项目旨在验证痕量（宏观和微观）测定的分析方法 动物诊断样品中的 6 元素、重金属和稀土元素污染。一个 7 2011-2012年开展的调查显示，全国共发生50多起污染事件 铜、硫、铅、砷、锌、硒等8种微量元素和重金属 9磷。此外，2009 年至 2012 年 FDA 召回的动物饲料包括 10 起来自锌、钾、铜和钼的污染事件。最后是稀土 事实证明，11 个要素对于追踪可疑的食品/饲料运输到特定地点非常有用 12 家制造商、供应商和地理区域。兽医诊断联盟 该提案中包括来自华盛顿州、爱达荷州、怀俄明州和犹他州的 13 个实验室 14 起与长期存在的矿物相关的动物污染事件的丰富经验 15 美国西部采矿业。所有实验室都将使用成熟的微波 16 消解和电感耦合等离子体质谱 (ICP-MS) 方法。正在关注 17 FDA指南，牵头实验室（华盛顿动物疾病诊断实验室- 18 分析科学实验室）将在动物体内产生均质且稳定的测试材料 19 研究过程中的饲料、动物组织（肝、肾、脑）、血液、牛奶和尿液（4 20年）用于大量元素、微量元素、重金属和稀土元素。对于每个 21 分析物方法、性能标准将记录准确度、精密度、选择性、 22 检测限、定量限、线性、范围、测量不确定度和 23 坚固性。怀俄明州和犹他州的联合实验室将使用标准化方法 24 项目期间开发的用于分析样品作为盲态未知物以确定 25 再现性和重复性。最终数据将使用 AOAC 2002 指南进行分析 26 化学方法验证和最终结果在整个 Vet-LIRN 中传达。的 合作协议的 27 项成果将增加所需的一套经过验证的方法 28 份动物诊断样本，以提高 FDA 的应对能力和能力 29 动物食品/饲料污染事件。 30

1 Project Summary: The FDA is currently lacking in standardized methods for ante mortem (live 2 animal) and post mortem analysis of animal diagnostic specimens potentially associated with 3 animal food/feed contamination events. To address this gap, existing FDA methodologies must 4 be extended to testing of new matrices such as milk, urine, blood, and tissues. The purpose of 5 this project is to validate analytical methods for determination of trace (macro and micro) 6 element, heavy metal, and rare earth element contamination in animal diagnostic samples. A 7 survey conducted in 2011-2012 revealed over 50 contamination events nationwide attributed to 8 trace elements and heavy metals such as copper, sulfur, lead, arsenic, zinc, selenium and 9 phosphorus. Furthermore, animal feed recalls by FDA from 2009-2012 have included 10 contamination events from zinc, potassium, copper, and molybdenum. Lastly, rare earth 11 elements have proved useful for tracing suspicious shipments of food/feed back to specific 12 manufacturers, suppliers, and geographical regions. The consortium of veterinary diagnostic 13 laboratories from Washington, Idaho, Wyoming, and Utah included in this proposal have 14 extensive experience animal contamination events associated with the long established mineral 15 mining industry in the western United States. All laboratories will use established microwave 16 digestion and Inductively Coupled Plasma Mass Spectrometer (ICP-MS) methods. Following 17 FDA guidelines, the lead laboratory (Washington Animal Disease Diagnostic Laboratory- 18 Analytical Sciences Laboratory) will generate homogeneous and stable test materials in animal 19 feed, animal tissues (liver, kidney, brain), blood, milk and urine over the course of the study (4 20 years) for macroelements, microelements, heavy metals, and rare earth elements. For each 21 analyte method, performance criteria will be documented for accuracy, precision, selectivity, 22 limit of detection, limit of quantification, linearity, range, measurement uncertainty and 23 ruggedness. Consortium laboratories in Wyoming and Utah will use standardize methods 24 developed during the project to analyze samples as blinded unknowns to determine 25 reproducibility and repeatability. Final data will be analyzed using AOAC 2002 guidelines for 26 validation of chemical methods and final results communicated throughout the Vet-LIRN. The 27 results of the cooperative agreement will increase the suite of validated methods needed for 28 animal diagnostic specimens in order to increase the capacity and capability of FDA to respond 29 to animal food/feed contamination events. 30