Chelab Srl, Lab R&D, via Fratta 25, 31023, Resana, TV, Italy.
J Mass Spectrom. 2012 Sep;47(9):1232-41. doi: 10.1002/jms.3074.
In the food industry, it is frequently necessary to check the quality of an ingredient to decide whether to use it in production and/or to have an idea of the final possible contamination of the finished product. The current need to quickly separate and identify relevant contaminants within different classes, often with legal residue limits on the order of 1-100 µg kg(-1), has led to the need for more effective analytical methods. With thousands of organic compounds present in complex food matrices, the development of new analytical solutions leaned towards simplified extraction/clean-up procedures and chromatography coupled with mass spectrometry. Efforts must also be made regarding the instrumental phase to overcome sensitivity/selectivity limits and interferences. For this purpose, high-resolution full scan analysis in mass spectrometry is an interesting alternative to the traditional tandem mass approach. A fast method for extracting and purifying bakery matrices was therefore developed and combined with the exploitation of ultra-high-pressure liquid chromatography (UHPLC) coupled to a Orbitrap Exactive™ high-resolution mass spectrometer (HRMS). Extracts of blank, naturally contaminated and fortified minicakes, prepared through a combined use of industrial and pilot plant production lines, were analyzed at different concentration levels (1-100 µg kg(-1)) of various contaminants: a limit of detection at 10 µg kg(-1) was possible for most of the analytes within all the categories analyzed, including pesticides, aflatoxins, trichothecene toxins and veterinary drugs. The application of accurate mass targeted screening described in this article demonstrates that current single-stage HRMS analytical instrumentation is well equipped to meet the challenges posed by chemical contaminants in the screening of both bakery raw materials and finished products.
在食品工业中，经常需要检查一种成分的质量，以决定是否在生产中使用它，以及了解最终产品可能受到的污染。目前需要快速分离和识别不同类别中的相关污染物，通常需要对法律残留限量为 1-100μg/kg（-1）的污染物进行分析。这导致了对更有效分析方法的需求。在复杂的食品基质中存在数千种有机化合物，新分析解决方案的开发倾向于简化提取/净化程序以及与质谱联用的色谱技术。在仪器方面也必须努力克服灵敏度/选择性限制和干扰。为此，质谱中的高分辨率全扫描分析是传统串联质谱方法的一种有趣替代方法。因此，开发了一种用于提取和净化烘焙基质的快速方法，并结合了超高效液相色谱（UHPLC）与轨道阱 Exactive™高分辨率质谱仪（HRMS）的联用。通过使用工业和中试生产线的组合制备空白、自然污染和加标迷你蛋糕的提取物，并在不同浓度水平（1-100μg/kg（-1））下分析了各种污染物：大多数分析物在所有分析类别中的检测限都达到了 10μg/kg（-1），包括农药、黄曲霉毒素、单端孢霉烯族毒素和兽药。本文描述的精确质量靶向筛选的应用表明，当前的单级 HRMS 分析仪器完全能够应对烘焙原料和成品中化学污染物筛选所带来的挑战。
