Malysheva Svetlana V, Goscinny Séverine, Malarvannan Govindan, Poma Giulia, Andjelkovic Mirjana, Voorspoels Stefan, Covaci Adrian, Van Loco Joris
a Food, Medicines and Consumer Safety , Scientific Institute of Public Health (WIV-ISP) , Brussels , Belgium.
b Toxicological Centre , University of Antwerp , Wilrijk , Belgium.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2018 Feb;35(2):292-304. doi: 10.1080/19440049.2017.1393110. Epub 2017 Oct 31.
An ultra-high performance liquid chromatography - tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated (in-house) for the quantification of selected brominated flame retardants (BFRs), including tetrabromobisphenol A (TBBPA), hexabromocyclododecanes (HBCDs), tetrabromobisphenol S (TBBPS) and bromophenols (BPs), in various food matrices. The sample preparation consisted of extraction of TBBPS with acidified acetonitrile followed by a fast dispersive solid-phase extraction (dSPE) clean-up and extraction of the other BFRs with a mixture of hexane and dichloromethane (1:1, v/v) with subsequent clean-up using acidified silica (44%, w/w). The limits of quantification of the method varied widely for the types of food matrices and the different classes of BFRs from 4 pg g wet weight (ww) to 8 ng g ww. For most of the analytes the apparent recovery was in the range 70-120%, and the method precision (under repeatability conditions) was below 20%. The method was successfully applied in proficiency testing exercises as well as for analysis of various food items. Only 25% of the collected food samples contained BFRs, with 4-bromophenol and α-HBCD as the only detected compounds. The contaminated foodstuffs were fish and eggs with concentrations in the range from 48 to 305 pg g ww.
建立了一种超高效液相色谱-串联质谱（UHPLC-MS/MS）方法并进行了内部验证，用于定量分析各类食品基质中选定的溴化阻燃剂（BFRs），包括四溴双酚A（TBBPA）、六溴环十二烷（HBCDs）、四溴双酚S（TBBPS）和溴酚（BPs）。样品制备过程包括用酸化乙腈萃取TBBPS，然后通过快速分散固相萃取（dSPE）净化，用己烷和二氯甲烷（1:1，v/v）的混合物萃取其他BFRs，随后用酸化硅胶（44%，w/w）净化。该方法的定量限因食品基质类型和不同种类的BFRs而有很大差异，从4 pg/g湿重（ww）到8 ng/g ww。对于大多数分析物，表观回收率在70%-120%范围内，方法精密度（在重复性条件下）低于20%。该方法成功应用于能力验证试验以及各类食品分析。所采集的食品样本中只有25%含有BFRs，仅检测到4-溴酚和α-HBCD这两种化合物。受污染的食品是鱼类和蛋类，浓度范围为48至305 pg/g ww。
