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气相色谱-质谱联用仪测定大气中痕量阻燃剂四溴双酚A

Trace determination of the flame retardant tetrabromobisphenol A in the atmosphere by gas chromatography-mass spectrometry.

作者信息

Xie Zhiyong, Ebinghaus Ralf, Lohmann Rainer, Heemken Olaf, Caba Armando, Püttmann Wilhelm

机构信息

GKSS Research Centre, Institute for Coastal Research, Department of Environmental Chemistry, Max-Planck-Str. 1, D-21502 Geesthacht, Germany.

出版信息

Anal Chim Acta. 2007 Feb 19;584(2):333-42. doi: 10.1016/j.aca.2006.10.062. Epub 2006 Nov 15.

Abstract

A simple and effective method has been developed for analysis of the flame retardant tetrabromobisphenol A (TBBPA) in environmental samples by using modified soxhlet extraction in combination with silica gel clean-up, derivatization with silylation reagent and gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring mode (SIM). Satisfactory recoveries were achieved for the large volume sampling, soxhlet extraction and silica gel clean-up. The overall recovery is 79+/-1%. The derivatization procedure is simple and fast, and produces stable TBBPA derivative. GC-MS with electronic impact (EI) ionization mode shows better detection power than using negative chemical ionization (NCI) mode. EI gives a method detection limit of 0.04 pgm(-3) and enables to determine trace TBBPA in ambient air in remote area. The method was successfully applied to the determination of TBBPA in atmospheric samples collected over land and coastal regions. The concentrations of TBBPA ranged from below the method detection limit (0.04 pgm(-3)) to 0.85 pgm(-3). A declining trend with increasing latitude was present from the Wadden Sea to the Arctic. The atmospheric occurrence of TBBPA in the Arctic is significant and might imply that TBBPA has long-range transport potential.

摘要

已开发出一种简单有效的方法,通过使用改进的索氏提取法结合硅胶净化、硅烷化试剂衍生化以及在选择离子监测模式(SIM)下的气相色谱-质谱联用(GC-MS)来分析环境样品中的阻燃剂四溴双酚A(TBBPA)。对于大体积采样、索氏提取和硅胶净化,回收率令人满意。总体回收率为79±1%。衍生化过程简单快速,并且能产生稳定的TBBPA衍生物。具有电子轰击(EI)电离模式的GC-MS比使用负化学电离(NCI)模式具有更好的检测能力。EI给出的方法检测限为0.04 pg m-3,能够测定偏远地区环境空气中的痕量TBBPA。该方法已成功应用于陆地和沿海地区采集的大气样品中TBBPA的测定。TBBPA的浓度范围从低于方法检测限(0.04 pg m-3)到0.85 pg m-3。从瓦登海到北极,随着纬度升高呈现下降趋势。TBBPA在北极大气中的存在较为显著,这可能意味着TBBPA具有长距离传输潜力。

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