Franchina Flavio Antonio, Lazzari Eliane, Scholl George, Focant Jean-François
Molecular Systems Research Unit, Faculty of Sciences, University of Liege, B-4000 Liege, Belgium.
Institute of Chemistry, Federal University of Rio Grande do Sul, 90040-060 Porto Alegre, Brazil.
Foods. 2019 Aug 1;8(8):302. doi: 10.3390/foods8080302.
Polychlorodibenzo--dioxins (PCDDs), polychloro-dibenzofurans (PCDFs), dioxin-like (DL), and non dioxin-like (NDL) polychlorinated biphenyls (PCBs) are currently regulated in food and feed within the European territory (EU 2017/644-771). The confirmatory methods of analysis for checking compliance with maximum levels (MLs) for these involve either the historically-established GC-magnetic sector high-resolution mass spectrometry (GC-HRMS) and, more recently, GC-triple quadrupole mass spectrometry operating in tandem mode (GC-QQQMS/MS). In this study, the performance of a novel triple quadrupole GC-QQQMS/MS system equipped with a programable temperature vaporization (PTV) injector was evaluated for the analysis of regulated PCDD/Fs and PCBs in food and feed. The MS analyzer was equipped with a titanium ionization chamber and a new short collision cell capable to accumulate and eject ions by means of very narrow pulses that allow to minimize the noise and to adapt accumulation times for sensitive multiple reaction monitoring (MRM). The analytical capability of the system was confronted by the strict requirements (selectivity, reproducibility, linearity, quant/qual MRM transitions, accuracy, robustness) set by the EU Regulation for a range of standards, quality control (QC) and food/feed samples. In this respect, the approach showed high precision (1.9-15% relative standard deviation (RSD) at low pg/µL) and accuracy (>80%, except for one hexa-CDD). The quantitative results were also compared to the most used GC-HRMS. In this case, comparable results in terms of single congener concentration basis and total toxic equivalent (TEQ) basis for PCDD/Fs and DL-PCBs were obtained for the QC samples analyzed.
多氯二苯并 - 二噁英（PCDDs）、多氯二苯并呋喃（PCDFs）、类二噁英（DL）和非类二噁英（NDL）多氯联苯（PCBs）目前在欧洲境内的食品和饲料中受到监管（欧盟2017/644 - 771）。用于检查这些物质是否符合最大限量（MLs）的确认性分析方法包括历史上确立的气相色谱 - 磁扇形高分辨率质谱法（GC - HRMS），以及最近的串联模式运行的气相色谱 - 三重四极杆质谱法（GC - QQQMS/MS）。在本研究中，对配备可编程温度汽化（PTV）进样器的新型三重四极杆GC - QQQMS/MS系统在分析食品和饲料中受监管的PCDD/Fs和PCBs方面的性能进行了评估。质谱分析仪配备了钛离子化室和一个新型短碰撞池，该碰撞池能够通过极窄的脉冲积累和喷射离子，从而将噪声降至最低，并根据灵敏的多反应监测（MRM）调整积累时间。该系统的分析能力与欧盟法规对一系列标准、质量控制（QC）和食品/饲料样品所设定的严格要求（选择性、重现性、线性、定量/定性MRM转换、准确性、稳健性）进行了对比。在这方面，该方法显示出高精度（低pg/μL时相对标准偏差（RSD）为1.9 - 15%）和高准确性（除一种六氯二噁英外，均>80%）。还将定量结果与最常用的GC - HRMS进行了比较。在这种情况下，对于所分析的QC样品，在单个同系物浓度基础和PCDD/Fs及DL - PCBs的总毒性当量（TEQ）基础方面获得了可比的结果。
