State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Shuangqing Road, Haidian District, Beijing 100085, China.
Talanta. 2010 Oct 15;82(5):1929-34. doi: 10.1016/j.talanta.2010.08.014. Epub 2010 Aug 19.
Hexabromocyclododecanes (HBCDs) and tris (2,3-dibromopropyl) isocyanurate (TBC) are both brominated flame retardants, and have been used throughout the world with subsequent concern for potential environment pollution. Here we describe the development of a method for the simultaneous determination of TBC and HBCD diastereoisomers in environmental matrices by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). The method recovery ranged from 81% to 93% and limits of detections (LODs) on column were 4.3 pg, 0.5 pg, 0.4 pg, 0.3 pg for TBC, α-HBCD, β-HBCD, and γ-HBCD, respectively, which showed high sensitivity compared to previous published methods. Compared to electrospray ionization (ESI), atmospheric pressure chemical ionization (APCI) was found to be a more sensitive, effective ionization mode for determination of HBCDs. This novel method was further validated by analyzing TBC and HBCDs in biotic and abiotic samples. The concentration ranges of TBC, α, β, γ-HBCD in sediment samples were 136.1-5884.6 ng/g, 9.0-1079.6 ng/g, 1.0-1161.7 ng/g, and 65.4-3964.2 ng/g, respectively. The concentration range for TBC, α-HBCD, β-HBCD, and γ-HBCD in common carp samples were 51.1-1899 ng/g, 21.6-1338 ng/g, <LOD-10.9 ng/g, and 1.4-101 ng/g, respectively.
六溴环十二烷（HBCDs）和三（2,3-二溴丙基）异氰脲酸酯（TBC）均为溴化阻燃剂，在全世界范围内广泛使用，随后人们开始关注其潜在的环境污染问题。在这里，我们描述了一种通过高效液相色谱串联质谱法（HPLC-MS/MS）同时测定环境基质中 TBC 和 HBCD 对映异构体的方法。该方法的回收率范围为 81%-93%，柱上检测限（LOD）分别为 TBC、α-HBCD、β-HBCD 和 γ-HBCD 的 4.3 pg、0.5 pg、0.4 pg 和 0.3 pg，与之前发表的方法相比，该方法具有较高的灵敏度。与电喷雾电离（ESI）相比，大气压化学电离（APCI）被发现是一种更灵敏、有效的电离模式，可用于测定 HBCDs。该新方法通过分析生物和非生物样品中的 TBC 和 HBCDs 得到了进一步验证。TBC、α、β、γ-HBCD 在沉积物样品中的浓度范围分别为 136.1-5884.6 ng/g、9.0-1079.6 ng/g、1.0-1161.7 ng/g 和 65.4-3964.2 ng/g。TBC、α-HBCD、β-HBCD 和 γ-HBCD 在鲤鱼样品中的浓度范围分别为 51.1-1899 ng/g、21.6-1338 ng/g、<LOD-10.9 ng/g 和 1.4-101 ng/g。
