Takahashi Shin, Sakai Shin-Ichi, Watanabe Isao
National Institute for Environmental Studies, Onogawa 16-2, Tsukuba, Ibaraki 305-8506, Japan.
Chemosphere. 2006 Jun;64(2):234-44. doi: 10.1016/j.chemosphere.2005.12.008. Epub 2006 Feb 3.
An intercalibration study on organobromine compounds has been conducted to evaluate the accuracy and reliability in the analysis of brominated flame retardants (BFRs) such as polybrominated diphenyl ethers (PBDEs) and their related compounds like polybrominated and monobromo-polychlorinated dibenzodioxins and -furans (PBDDs/DFs, MoBPCDDs/DFs). This paper reports the results for these compounds in 'Mixed Standard Solutions' and 'Air-Dried Sediment'. The relative standard deviations (RSDs) for PBDEs, PBDDs/DFs and MoBPCDDs/DFs in mixed standard solutions ranged from 9% to 24%, 4% to 20% and 8% to 27%, respectively. The results of this study are better than those reported in earlier international interlaboratory studies due to general improvement in analytical methods and an increasing number of available authentic standards, particularly for PBDEs. In the analysis for higher brominated compounds such as octabromodibenzodioxin, the participants were advised to optimize the calibration curves befitting the range of concentrations found in samples because variation of relative response factors was noted. The results for 'Air-Dried Sediment' were also reasonable with RSDs from 10% to 38% for PBDEs, 8% to 38% for PBDDs/DFs and 17% to 36% for MoBPCDDs/DFs. In the sediment sample, possible errors in the sample pretreatment and/or interference by other compounds/impurities were indicated. The concentrations of pentabromodiphenylether, BDE100, varied more than the other PBDE isomers due to its poor separation in some chromatographic conditions. In addition, interference by PBDEs was observed in the analysis for PBDFs. Potential degradation/secondary formulation of PBDEs and PBDFs during the Soxhlet extraction were suggested when copper powder was added into the sediment samples. Inspite of these observations, the results in this study are better than those reported in other interlaboratory studies due to the advice given to participants for improving the results. Compared with the results for PCDDs/DFs (5-23% RSDs) and Co-PCBs (6-24% RSDs), the RSDs for most of the organobromine compounds were high, indicating an immature QA/QC approach for the analysis of PBDEs and related compounds in comparison to common chlorinated dioxins.
已开展一项关于有机溴化合物的比对研究，以评估分析溴化阻燃剂（BFRs）（如多溴二苯醚（PBDEs））及其相关化合物（如多溴和单溴多氯二苯并二恶英及二苯并呋喃（PBDDs/DFs、MoBPCDDs/DFs））时的准确性和可靠性。本文报告了这些化合物在“混合标准溶液”和“风干沉积物”中的检测结果。混合标准溶液中PBDEs、PBDDs/DFs和MoBPCDDs/DFs的相对标准偏差（RSDs）分别为9%至24%、4%至20%和8%至27%。由于分析方法的普遍改进以及可用的真实标准品数量增加，尤其是对于PBDEs，本研究的结果优于早期国际实验室间研究报告的结果。在分析八溴二苯并二恶英等高溴化化合物时，建议参与者优化校准曲线以适应样品中发现的浓度范围，因为注意到相对响应因子存在变化。“风干沉积物”的结果也较为合理，PBDEs的RSDs为10%至38%，PBDDs/DFs为8%至38%，MoBPCDDs/DFs为17%至36%。在沉积物样品中，指出了样品预处理中可能存在的误差和/或其他化合物/杂质的干扰。五溴二苯醚（BDE100）的浓度变化比其他PBDE异构体更大，这是因为在某些色谱条件下其分离效果较差。此外，在分析PBDFs时观察到PBDEs的干扰。当向沉积物样品中加入铜粉时，提示在索氏提取过程中PBDEs和PBDFs可能发生降解/二次形成。尽管有这些观察结果，但由于向参与者提供了改进结果的建议，本研究的结果仍优于其他实验室间研究报告的结果。与多氯二苯并二恶英及呋喃（PCDDs/DFs）（RSDs为5 - 23%）和共平面多氯联苯（Co - PCBs）（RSDs为6 - 24%）的结果相比，大多数有机溴化合物的RSDs较高，这表明与常见的氯代二恶英相比，PBDEs及其相关化合物分析的质量保证/质量控制方法尚不成熟。
