US Department of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 East Mermaid Lane, Wyndmoor, PA, 19038, USA.
US Department of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 East Mermaid Lane, Wyndmoor, PA, 19038, USA.
Anal Chim Acta. 2022 Oct 16;1230:340400. doi: 10.1016/j.aca.2022.340400. Epub 2022 Sep 15.
Instances of food contamination with per- and polyfluoroalkyl substances (PFAS) continue to occur globally, but sample preparation and analytical methods are quite limited and often monitor for a small percentage of known PFAS. This study aimed to evaluate, validate, and compare performance of two instruments with the recently developed "quick, easy, cheap, effective, rugged, safe, efficient, and robust" (QuEChERSER) sample preparation mega-method - a method developed to monitor chemicals over a broad range of physicochemical properties. Initial evaluation of the QuEChERSER mega-method for determination of PFAS in food demonstrated recoveries, matrix interferences, and co-extractive removal comparable to (or better than) US Food and Drug Administration (FDA) and USDA Food Safety and Inspection Service (FSIS) methods. Subsequent validation of QuEChERSER in beef, catfish, chicken, pork, liquid eggs, and powdered eggs on a high-resolution mass spectrometer achieved acceptable recoveries (70-120%) and precision (RSDs ≤20%) for all 33 target analytes at the 1 and 5 ng g levels and 67-88% of analytes at the 0.1 ng g level, depending on the matrix. Additional validation was performed by tandem mass spectrometry on a triple quadrupole instrument. This approach provided no non-detects and better recoveries at the 0.1 ng g level than the HRMS method but exhibited more variability at 1 and 5 ng g spiking levels. Analysis of NIST SRMs 1946 and 1947 gave accuracies of 70-117%. These results demonstrate the capability of combining PFAS analysis with a mega-method previously validated for 350 analytes, while collecting non-target data for future retrospective analysis of emerging alternatives with a high-resolution mass spectrometry method.
食品中全氟和多氟烷基物质(PFAS)的污染实例在全球范围内仍时有发生,但样品制备和分析方法相当有限,而且通常只能监测一小部分已知的 PFAS。本研究旨在评估、验证和比较两种仪器与最近开发的“快速、简便、廉价、有效、耐用、安全、高效、强大”(QuEChERSER)样品制备大方法的性能 - 该方法旨在监测广泛理化性质的化学品。初步评估 QuEChERSER 用于食品中 PFAS 的测定方法表明,回收率、基质干扰和共提取去除与美国食品和药物管理局(FDA)和美国农业部食品安全检验局(FSIS)方法相当(或更好)。随后在高分辨质谱仪上对牛肉、鲶鱼、鸡肉、猪肉、液态蛋和蛋粉进行 QuEChERSER 的后续验证,在 1 和 5ng/g 水平和 67-88%的基质水平下,所有 33 种目标分析物的回收率(70-120%)和精密度(RSDs≤20%)均可接受,取决于基质。在三重四极杆仪器上通过串联质谱法进行了额外的验证。与 HRMS 方法相比,该方法在 0.1ng/g 水平下提供了更多的非检出物和更好的回收率,但在 1 和 5ng/g 加标水平下表现出更大的变异性。对 NIST SRM 1946 和 1947 的分析结果表明,准确度为 70-117%。这些结果表明,将 PFAS 分析与以前针对 350 种分析物验证的大方法相结合,同时使用高分辨质谱法收集非目标数据,以便对新兴替代品进行未来回溯分析,这是可行的。