Optimization and development of analytical methods for the determination of new brominated flame retardants and polybrominated diphenyl ethers in sediments and suspended particulate matter
Optimization and development of analytical methods for the determination of new brominated flame retardants and polybrominated diphenyl ethers in sediments and suspended particulate matter
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DOI：
10.1007/s00216-011-4807-8
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发表时间：
2011-05-01
影响因子：
4.3
通讯作者：
de Boer, J.
中科院分区：
文献类型：
--
作者：
Lopez, P.;Brandsma, S. A.;de Boer, J.
随着有关溴化阻燃剂的立法更加严格，预计将有越来越多的替代品取代多溴二苯醚。因此，开发和优化分析方法，使其能够识别和量化，具有至关重要的意义。本工作描述了一种分析方法的优化，以测定沉积物和悬浮颗粒物中的五溴氯环己烷、四溴邻氯甲苯、2，3，5，6-四溴对二甲苯、四溴邻苯二甲酸酐、2，3，4，5，6-五溴甲苯、三（2，3-二溴丙基）磷酸盐、十溴二苯基乙烷和1，2-双（2，4，6-三溴苯氧基）乙烷以及多溴二苯醚。该方法包括加压液体萃取，然后是三个净化步骤（凝胶渗透色谱法和在OasisTM HLB和硅胶柱上的固相萃取）。采用气相色谱-质谱法，使用电子捕获负化学电离，用于最终分析。该方法的回收率> 85%。该方法被应用于沉积物和悬浮颗粒物样品从不同的位置在西斯海尔德河口（荷兰）。据我们所知，这是第一次在文献中报道添加阻燃剂2，3，5，6-四溴-对二甲苯，3，4，5，6-四溴-邻氯甲苯和2，3，4，5，6-五溴氯环己烷的出现。这些新型阻燃剂的浓度范围为0.05至0.30微克/千克干重。
With more stringent legislation on brominated flame retardants, it is expected that increasing amounts of substitutes would replace polybrominated diphenylethers (PBDEs). Therefore, the development and optimization of analytical methodologies that allow their identification and quantification are of paramount relevance. This work describes the optimization of an analytical procedure to determine pentabromochlorocyclohexane, tetrabromo-o-chlorotoluene, 2,3,5,6-tetrabromo-p-xylene, tetrabromophthalic anhydride, 2,3,4,5,6-pentabromotoluene, tris(2,3-dibromopropyl)phosphate, decabromodiphenylethane and 1,2-bis(2,4,6-tribromophenoxy)ethane together with PBDEs in sediments and in suspended particulate matter. This method comprises a pressurized liquid extraction followed by three cleanup steps (gel permeation chromatography and solid phase extraction on Oasis (TM) HLB and on silica cartridges). Gas chromatography-mass spectrometry, using electron capture negative chemical ionization, is used for the final analysis. The proposed method provides recoveries > 85%. The method was applied to sediment and suspended particulate matter samples from different locations in the Western Scheldt estuary (the Netherlands). To the best of our knowledge, this is the first time that the occurrence of the additive flame retardants 2,3,5,6-tetrabromo-p-xylene, 3,4,5,6-tetrabromo-o-chlorotoluene and 2,3,4,5,6-pentabromochlorocyclohexane is reported in the literature. The concentrations of these new flame retardants ranged from 0.05 to 0.30 mu g/kg dry weight.