Phillips Melissa M, Seal Tomás M López, Ness Jennifer M, Zhang Kai
U.S. National Institute of Standards and Technology (NIST), Chemical Sciences Division, Gaithersburg, MD.
U.S. National Institute of Standards and Technology (NIST), Chemical Sciences Division, Charleston, SC.
J AOAC Int. 2019 Nov 1;102(6):1642-1650. doi: 10.5740/jaoacint.19-0109. Epub 2019 Jun 17.
Matrix-matched reference materials (RMs) are critical for adequate quality assurance of extraction, digestion, separation, and/or detection processes for analytes of interest in foods and dietary supplements. The accurate determination of mycotoxins in foods is an international concern. While RMs for mycotoxins are available from a variety of RM producers, these mainly address a single mycotoxin or group of mycotoxins and therefore require the use of multiple RMs for multitarget methods. To address the increasing needs of laboratories moving toward LC-MS-based multimycotoxin analysis, the U.S. National Institute of Standards and Technology (NIST) collaborated with the U.S. Food and Drug Administration (FDA) to produce a naturally incurred RM for multiple mycotoxins in corn. Homogeneity of the RM has been assessed using a stratified random sampling of the final product based on mycotoxin mass fractions measured by the FDA and NIST. Multiple sample sizes were evaluated to maximize homogeneity in the obtained results. The mycotoxin levels in the final materials have been evaluated via interlaboratory comparison and isotope dilution LC-tandem MS measurements made at the FDA and NIST. The final value assignment combined results from these data sets. The study successfully developed a certified RM, SRM 1565 Mycotoxins in Corn, and a workflow for the future development of multimycotoxin RMs in different matrices.
基质匹配参考物质(RMs)对于食品和膳食补充剂中目标分析物的提取、消化、分离和/或检测过程的充分质量保证至关重要。食品中霉菌毒素的准确测定是一个国际关注的问题。虽然有多种RM生产商提供霉菌毒素的参考物质,但这些主要针对单一霉菌毒素或一组霉菌毒素,因此对于多目标方法需要使用多种参考物质。为了满足实验室对基于液相色谱 - 质谱联用的多霉菌毒素分析日益增长的需求,美国国家标准与技术研究院(NIST)与美国食品药品监督管理局(FDA)合作,生产了一种玉米中多种霉菌毒素的天然污染参考物质。已根据FDA和NIST测定的霉菌毒素质量分数,对最终产品进行分层随机抽样,评估了参考物质的均匀性。评估了多个样本量,以最大限度地提高所得结果的均匀性。最终材料中的霉菌毒素水平已通过实验室间比对以及在FDA和NIST进行的同位素稀释液相色谱 - 串联质谱测量进行了评估。最终的值赋值结合了这些数据集的结果。该研究成功开发了一种有证参考物质,即玉米中的SRM 1565霉菌毒素,以及一种用于未来不同基质中多霉菌毒素参考物质开发的工作流程。