De Dominicis Emiliano, Commissati Italo, Gritti Elisa, Catellani Dante, Suman Michele
a R&D Department Chelab-Silliker , Mérieux Nutriscience Company , Resana (TV) , Italy.
b Food Research Labs Department, Barilla SpA , Parma , Italy.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2015;32(10):1617-27. doi: 10.1080/19440049.2015.1061703. Epub 2015 Jul 28.
In addition to 'traditional' multi-residue and multi-contaminant multiple reaction monitoring (MRM) mass spectrometric techniques devoted to quantifying a list of targeted compounds, the global food industry requires non-targeted methods capable of detecting other possible potentially hazardous compounds. Ultra-high-performance liquid chromatography combined with a single-stage Orbitrap high-resolution mass spectrometer (UHPLC-HRMS Exactive™-Orbitrap Technology) was successfully exploited for the complete selective and quantitative determination of 33 target compounds within three major cross categories (pesticides, antibiotics and mycotoxins) in bakery matrices (specifically milk, wheat flour and mini-cakes). Resolution was set at 50 000 full width at half maximum (FWHM) to achieve the right compromise between an adequate scan speed and selectivity, allowing for the limitations related to the necessary generic sample preparation approach. An exact mass with tolerance of 5 ppm and minimum peak threshold of 10 000 units were fixed as the main identification conditions, including retention time and isotopic pattern as additional criteria devoted to greatly reducing the risk of false-positive findings. The full validation for all the target analytes was performed: linearity, intermediate repeatability and recovery (28 analytes within 70-120%) were positively assessed; furthermore, limits of quantification between 5 and 100 µg kg(-1) (with most of the analytes having a limit of detection below 6 µg kg(-1)) indicate good performance, which is compatible with almost all the regulatory needs. Naturally contaminated and fortified mini-cakes, prepared through combined use of industrial and pilot plant production lines, were analysed at two different concentration levels, obtaining good overall quantitative results and providing preliminary indications of the potential of full-scan HRMS cluster analysis. The effectiveness of this analytical approach was also tested in terms of the formulation of hypotheses for the identification of other analytes not initially targeted which can have toxicological implications (e.g. 3-acetyl-deoxynivalenol and deoxynivalenol-3-glucoside), opening a window on retrospective investigation perspectives in food safety laboratories.
除了用于定量一系列目标化合物的“传统”多残留和多污染物多反应监测（MRM）质谱技术外，全球食品行业还需要能够检测其他可能潜在有害化合物的非靶向方法。超高效液相色谱结合单级轨道阱高分辨率质谱仪（UHPLC-HRMS Exactive™-轨道阱技术）成功用于在烘焙基质（具体为牛奶、小麦粉和小蛋糕）中对三大交叉类别（农药、抗生素和霉菌毒素）内的33种目标化合物进行完整的选择性和定量测定。分辨率设定为50000半高宽（FWHM），以便在适当的扫描速度和选择性之间取得恰当平衡，同时考虑到与必要的通用样品制备方法相关的局限性。将5 ppm的质量精度公差和10000单位的最小峰阈值作为主要鉴定条件，包括保留时间和同位素模式作为额外标准，以大幅降低假阳性结果的风险。对所有目标分析物进行了全面验证：线性、中间重复性和回收率（28种分析物在70%-120%之间）得到了积极评估；此外，5至100 μg kg⁻¹的定量限（大多数分析物的检测限低于6 μg kg⁻¹）表明性能良好，几乎符合所有监管要求。通过联合使用工业和中试生产线制备的天然污染和加标小蛋糕，在两个不同浓度水平下进行了分析，获得了良好的总体定量结果，并为全扫描HRMS聚类分析的潜力提供了初步指示。还从为鉴定其他最初未靶向但可能具有毒理学意义的分析物（如3-乙酰脱氧雪腐镰刀菌烯醇和脱氧雪腐镰刀菌烯醇-3-葡萄糖苷）提出假设的角度测试了这种分析方法的有效性，为食品安全实验室的回顾性调查前景打开了一扇窗口。
