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同时液相色谱-串联质谱法分析法国母乳中的溴系阻燃剂(四溴双酚 A 和六溴环十二烷对映异构体)。

Simultaneous liquid chromatography-tandem mass spectrometry analysis of brominated flame retardants (tetrabromobisphenol A and hexabromocyclododecane diastereoisomers) in French breast milk.

机构信息

Université Paris-Est, ANSES, Laboratory for Food Safety, F-94700, Maisons-Alfort, France.

Université Paris-Est, ANSES, Laboratory for Food Safety, F-94700, Maisons-Alfort, France.

出版信息

Chemosphere. 2017 Nov;186:762-769. doi: 10.1016/j.chemosphere.2017.08.020. Epub 2017 Aug 8.

Abstract

TBBPA and HBCDs are the two classes of flame retardants that are still allowed for use by the European Commission. In May 2013, HBCDs were listed as Persistent Organic Pollutants under the Stockholm Convention, and they were banned with an exemption on EPS/XPS for cavity wall insulation. This study describes the development and optimisation of a rapid LC-ESI-MS/MS method using isotopic dilution quantification including a simplified extraction step using a mixture of solvents and sulphuric acid hydrolysis followed by the one-shot analysis of TBBPA and each of the α-, β- and γ-HBCD diastereoisomers. The limits of detection and quantification (LOD and LOQ) were 0.5 and 2.5 ng g (lipid weight, lw) for TBBPA and HBCD diastereoisomers, respectively. The method was applied to analyse 106 samples of individual mature breast milk. TBBPA was quantified in 42% of these samples within a range of <LOQ to 15.1 ng g lw. HBCD diastereoisomers were quantified in 8%, 3% and 3% of the collected samples for α-, β- and γ-HBCDs, respectively. The α-form was predominant in each quantifiable breast milk sample. The rapid newly developed LC-MS/MS method appears to be suitable for simultaneously analysing and quantifying TBBPA and HBCDs (three isomers) in human breast milk with the aim of establishing BFR multi-contamination profiles of breast milk samples.

摘要

TBBPA 和 HBCDs 是欧盟委员会仍允许使用的两类阻燃剂。2013 年 5 月,HBCDs 被斯德哥尔摩公约列为持久性有机污染物,除了用于空腔壁绝缘的 EPS/XPS 之外,HBCDs 被禁止使用。本研究描述了一种快速 LC-ESI-MS/MS 方法的开发和优化,该方法采用同位素稀释定量法,包括使用溶剂混合物和硫酸水解的简化提取步骤,然后一次性分析 TBBPA 和每种 α-、β-和 γ-HBCD 非对映异构体。检测限和定量限 (LOD 和 LOQ) 分别为 0.5 和 2.5 ng g(脂质重量,lw)用于 TBBPA 和 HBCD 非对映异构体。该方法应用于分析 106 份个体成熟母乳样本。在这些样本中,42%的样本中定量了 TBBPA,范围为<LOQ 至 15.1 ng g lw。在收集到的样本中,α-HBCD、β-HBCD 和 γ-HBCD 的定量分别为 8%、3%和 3%。在每个可定量的母乳样本中,均以 α 形式为主。新开发的快速 LC-MS/MS 方法似乎适用于同时分析和定量人乳中的 TBBPA 和 HBCDs(三种异构体),旨在建立母乳样本中 BFR 多污染图谱。

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