Gonzalez-Gago Adriana, Pröfrock Daniel, Prange Andreas
Department Marine Bioanalytical Chemistry, Helmholtz Zentrum Geesthacht - Zentrum für Material und Küstenforschung, Institute of Coastal Research, Max-Planck Str. 1, 21502, Geesthacht, Germany.
Anal Bioanal Chem. 2015 Oct;407(26):8009-18. doi: 10.1007/s00216-015-8973-y. Epub 2015 Aug 29.
The Water Framework Directive (WFD) includes some polybrominated diphenyl ethers (PBDEs) in the list of priority substances that must be measured in surface waters at very low concentrations. The typical approaches applied to the determination of PBDEs in environmental samples might not meet the demanding requirements of the WFD. In this work, the instrumental capabilities of the mass-spectrometry (MS) techniques most frequently used in the determination of PBDEs, namely gas chromatography-negative-chemical-ionisation MS (GC-NCI MS) and GC-electrospray-ionisation tandem MS (EI MS-MS), are evaluated in comparison with highly sensitive GC-inductively-coupled-plasma MS (ICP-MS) for the reliable determination of PBDEs according to the WFD. Three analytical methods based on the liquid-liquid extraction of water samples and measurement of the extracts by GC-NCI MS, GC-EI MS-MS, or GC-ICP-MS are described. The priority PBDEs were quantified in different types of water sample by means of isotope-dilution mass spectrometry (IDMS) using (81)Br-labelled or (13)C-labelled PBDEs spikes, depending on the selected ionisation source. The three proposed methods met the requirements of the European legislation in terms of LOQs and expanded uncertainties. The determination method using (81)Br-labelled PBDEs and GC-ICP-MS had the highest sensitivity and the lowest instrumental limits of detection and expanded uncertainties.
《水框架指令》（WFD）将一些多溴二苯醚（PBDEs）列入了优先物质清单，这些物质必须在地表水中以极低浓度进行测量。用于测定环境样品中多溴二苯醚的典型方法可能无法满足《水框架指令》的严格要求。在这项工作中，与高灵敏度的气相色谱 - 电感耦合等离子体质谱法（GC - ICP - MS）相比，评估了在多溴二苯醚测定中最常用的质谱（MS）技术的仪器性能，即气相色谱 - 负化学电离质谱法（GC - NCI MS）和气相色谱 - 电喷雾电离串联质谱法（EI MS - MS），以便根据《水框架指令》可靠地测定多溴二苯醚。描述了三种基于水样液 - 液萃取并通过GC - NCI MS、GC - EI MS - MS或GC - ICP - MS测量提取物的分析方法。根据所选电离源，使用（81）Br标记或（13）C标记的多溴二苯醚加标，通过同位素稀释质谱法（IDMS）对不同类型水样中的优先多溴二苯醚进行定量。所提出的三种方法在最低定量限（LOQs）和扩展不确定度方面符合欧洲法规要求。使用（81）Br标记的多溴二苯醚和GC - ICP - MS的测定方法具有最高灵敏度以及最低的仪器检测限和扩展不确定度。
