REQUIMTE/LAQV, Instituto Superior de Engenharia do Porto, Instituto Politécnico do Porto, Rua Dr° António Bernardino de Almeida, 431, 4200-072 Porto, Portugal.
Faculty of Engineering Technology, Hasselt University, KU Leuven, 3590 Diepenbeek, Belgium.
J Agric Food Chem. 2020 Mar 11;68(10):3260-3266. doi: 10.1021/acs.jafc.9b07041. Epub 2020 Feb 28.
One of the main challenges for analytical laboratories and food safety authorities is the control of food contaminants hazardous to human health. For the first time, a simple, fast, and cost-effective sample preparation method is proposed as an extraction technique to determine 12 brominated flame retardants (BFRs) (seven polybrominated diphenyl ether (PBDE) congeners and five novel BFRs) in cultivars. Different QuEChERS and dispersive solid-phase extract (d-SPE) sorbent compositions were evaluated in terms of recovery and matrix effects. The best results were obtained with citrate-buffered version QuEChERS and a cleanup step, with 150 mg of MgSO, 50 mg of primary secondary amine (PSA), 50 mg of C18, and 5 mg of carbon. The limit of detection (LOD) was between 1.4 and 9.3 μg/kg and > 0.99. Recoveries and matrix effects were between 66 and 104% and 0.58 and 2.18, respectively. The relative standard deviations from repeatability and reproducibility studies and estimation of measurement uncertainty were lower than 20%. Gas chromatography coupled with a mass spectrometer was used to confirm the presence of BFRs in the samples. Novel BFRs were detected lower than the LOD.
对于分析实验室和食品安全当局来说，主要挑战之一是控制对人类健康有害的食品污染物。首次提出了一种简单、快速且具有成本效益的样品制备方法，作为提取技术，用于测定 品种中 12 种溴化阻燃剂（BFRs）（七种多溴联苯醚（PBDE）同系物和五种新型 BFRs）。从回收率和基质效应两方面评估了不同的 QuEChERS 和分散固相萃取（d-SPE）吸附剂组成。使用柠檬酸缓冲的 QuEChERS 版本和净化步骤可获得最佳结果，其中包含 150mg 的 MgSO、50mg 的初级/次级胺（PSA）、50mg 的 C18 和 5mg 的碳。检出限（LOD）在 1.4 至 9.3μg/kg 之间，相关系数>0.99。回收率和基质效应分别在 66%至 104%和 0.58 至 2.18 之间。重复性和再现性研究以及测量不确定度估计的相对标准偏差均低于 20%。采用气相色谱-质谱联用仪确认样品中存在 BFRs。新型 BFRs 的检出限低于 LOD。
