Yu Zhiqiang, Peng Ping'an, Sheng Guoying, Fu Jiamo
State Key laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, China.
J Chromatogr A. 2008 May 9;1190(1-2):74-9. doi: 10.1016/j.chroma.2008.02.082. Epub 2008 Mar 2.
Hexabromocyclododecanes (HBCDs), used as additive brominated flame retardants, are of high concern due to their widespread use and increasing levels in various environmental systems. High-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (LC-MS/MS) was developed for the determination of HBCD diastereoisomers. A detailed study was carried out to optimize the composition of the mobile phase involving methanol/acetonitrile/water, and the values of MS/MS parameters. It was found that the mobile phase could simultaneously affect the chromatographic separation and sensitivity. The instrumental limits of detection (LODs) on column in this study were 0.5, 0.3 and 0.3 pg for alpha-HBCD, beta-HBCD and gamma-HBCD, respectively. The effects of extracted matrix components on HBCD determination were investigated by spiking air and soil sample extracts with three 13C-labelled individual stereoisomers. The results indicated that the responses of the HBCD analysis in air and soils were not significantly affected by matrix effects. The method reported here was further applied to the air and soil samples. Three HBCD diastereoisomers were detected in all the air and soil samples, with levels ranging from 1.2 to 1.8 pg/m3 and 1.7 to 5.6 ng/g dry weight, respectively.
六溴环十二烷（HBCDs）作为添加型溴化阻燃剂，因其广泛使用且在各种环境系统中的含量不断增加而备受关注。开发了高效液相色谱-电喷雾电离串联质谱法（LC-MS/MS）用于测定HBCD非对映异构体。开展了详细研究以优化包含甲醇/乙腈/水的流动相组成以及MS/MS参数值。发现流动相可同时影响色谱分离和灵敏度。本研究中柱上仪器检测限（LOD）对于α-HBCD、β-HBCD和γ-HBCD分别为0.5、0.3和0.3 pg。通过向空气和土壤样品提取物中加入三种13C标记的单一立体异构体来研究提取的基质成分对HBCD测定的影响。结果表明空气和土壤中HBCD分析的响应不受基质效应的显著影响。此处报道的方法进一步应用于空气和土壤样品。在所有空气和土壤样品中均检测到三种HBCD非对映异构体，含量分别在1.2至1.8 pg/m3和1.7至5.6 ng/g干重范围内。
