US Food and Drug Administration, Northeast Food and Feed Laboratory, Office of Regulatory Affairs, 158-15 Liberty Avenue, Jamaica, NY 11433, USA.
U.S. Food and Drug Administration, Center for Food Safety and Applied Nutrition, 5001 Campus Drive, HFS 716, College Park, MD 20740, USA.
J AOAC Int. 2024 Jul 4;107(4):632-640. doi: 10.1093/jaoacint/qsae029.
An interlaboratory study was conducted at the U.S. Food and Drug Administration's (FDA) Northeast Food and Feed Laboratory (NFFL) and the Center for Food Safety and Applied Nutrition (CFSAN) with the purpose to expand FDA Elemental Analysis Manual (EAM) method 4.7 (Inductively Coupled Plasma-Mass Spectrometric Determination of Arsenic, Cadmium, Chromium, Lead, Mercury, and Other Elements in Food Using Microwave Assisted Digestion) to include new analytes.
The goal of the study was to demonstrate the performance of FDA EAM method 4.7 when analyzing new analytes cobalt (Co), strontium (Sr), thallium (Tl), tin (Sn), uranium (U), and vanadium (V). This analyte extension method validation of EAM 4.7 for six additional elements, Co, Sr, Tl, Sn, U, and V, followed all guidelines for a Level 2 or single-laboratory validation and met all acceptance criteria for analyte extensions as per the Guidelines for the Validation of Chemical Methods.
As per EAM 4.7, this study followed the procedures and used specified equipment operated under recommended conditions. The analyte extension method validation was performed in accordance with protocol and with no deviations.
All quality control (QC) requirements for this analyte extension method validation of EAM 4.7 passed as evidenced by the analytical data. The results presented demonstrate accuracy, linearity, and precision by successful analyses of method blanks, matrix spikes, unfortified test samples, and reference materials. The data analyzed met each of the validation requirements for each analyte in all representative matrixes.
The study showed that the new analytes performed satisfactorily using EAM 4.7 for total acidic extractable elemental analysis of food according to FDA's guidelines.
The method met or exceeded the performance criteria.
本研究在美国食品药品监督管理局（FDA）东北食品和饲料实验室（NFFL）和食品安全与应用营养中心（CFSAN）进行了实验室间研究，旨在扩展 FDA 元素分析手册（EAM）方法 4.7（微波辅助消解的食物中砷、镉、铬、铅、汞和其他元素的电感耦合等离子体质谱法测定），以包括新的分析物。
该研究的目标是证明 FDA EAM 方法 4.7 在分析新分析物钴（Co）、锶（Sr）、铊（Tl）、锡（Sn）、铀（U）和钒（V）时的性能。EAM 4.7 对这六种额外元素（Co、Sr、Tl、Sn、U 和 V）的分析物扩展方法验证符合二级或单实验室验证的所有指南，并符合化学方法验证指南中规定的分析物扩展的所有验收标准。
根据 EAM 4.7，本研究按照程序进行，并使用指定的设备，按照推荐的条件操作。根据协议进行分析物扩展方法验证，没有偏差。
所有的质量控制（QC）要求都通过了 EAM 4.7 分析物扩展方法验证的分析数据证明了这一点。结果表明，成功分析方法空白、基质加标、未加标测试样品和参考物质，证明了该方法的准确性、线性和精密度。在所有代表性基质中，分析数据都符合每种分析物的每个验证要求。
该研究表明，根据 FDA 的指南，使用 EAM 4.7 进行食物总酸性可提取元素分析时，新的分析物表现令人满意。
该方法满足或超过了性能标准。
