Institute of Chemical Technology, Prague, Faculty of Food and Biochemical Technology, Department of Analysis and Nutrition, Technicka 3, 166 28 Prague, Czech Republic.
Talanta. 2013 Dec 15;117:318-25. doi: 10.1016/j.talanta.2013.08.040. Epub 2013 Aug 30.
In the present study, a novel analytical approach for the simultaneous determination of 18 perfluoroalkyl substances (PFASs) and 11 brominated flame retardants (BFRs) including their hydroxylated metabolites and brominated phenols has been developed and validated for breast milk and infant formula. The sample preparation procedure based on extraction using acetonitrile and subsequent purification by dispersive solid-phase extraction (d-SPE) employing C18 sorbent is rapid, simple and high-throughput. Ultra-high performance liquid chromatography (UHPLC) interfaced with a tandem mass spectrometry (MS/MS) was employed for the identification/quantification of these compounds. The method recoveries of target compounds for both matrices ranged from 80% to 117% with relative standard deviations lower than 28% and quantification limits in the range of 3-200 pg/mL for milk and 5-450 pg/g for infant formula. Within the pilot study, the new method was used for the analysis of PFASs and BFRs in 50 human breast milks and six infant formulas. In the breast milk samples the total contents of PFASs and BFRs were in the range of 38-279 and 45-16,200 pg/mL, respectively. The most abundant PFASs detected in all tested breast milk samples were perfluorooctanoic acid (PFOA) and perfluorooctanesulfonate (PFOS), the latter contaminant was present not only as a linear form but also as a branched isomers. The incidence of BFRs was lower, the only representatives of this group, tetrabromobiphenol A (TBBPA) and α-hexabromocyclododecane (α-HBCD), were detected in less than 30% of breast milk samples. None of the infant formulas contained BFRs, traces of either PFOS, PFOA or PFNA were found in three samples.
在本研究中，建立并验证了一种用于同时测定母乳和婴儿配方奶中 18 种全氟烷基物质（PFASs）和 11 种溴代阻燃剂（BFRs）及其羟基代谢物和溴代酚的新型分析方法。该方法基于乙腈提取，随后采用 C18 吸附剂的分散固相萃取（d-SPE）进行净化，具有快速、简单和高通量的特点。超高效液相色谱（UHPLC）与串联质谱（MS/MS）联用用于这些化合物的鉴定/定量。对于两种基质，目标化合物的方法回收率在 80%至 117%之间，相对标准偏差低于 28%，定量限在 3-200 pg/mL 范围内（对于母乳）和 5-450 pg/g 范围内（对于婴儿配方奶）。在试点研究中，该新方法用于分析 50 个人乳样本和 6 个婴儿配方样本中的 PFASs 和 BFRs。在母乳样本中，PFASs 和 BFRs 的总含量分别在 38-279 和 45-16,200 pg/mL 范围内。在所测试的所有母乳样本中，检测到的最丰富的 PFASs 是全氟辛酸（PFOA）和全氟辛烷磺酸（PFOS），后者不仅以线性形式存在，还以支链异构体形式存在。BFRs 的检出率较低，该组的唯一代表物四溴双酚 A（TBBPA）和α-六溴环十二烷（α-HBCD）仅在不到 30%的母乳样本中检出。婴儿配方奶中均未检出 BFRs，在三个样本中检测到痕量的 PFOS、PFOA 或 PFNA。
