中文摘要：

建立了一种同时测定沉积物中不同赋存形态的多溴联苯醚（PBDEs）和四溴双酚A（TBBPA）的分析方法。样品由等体积的丙酮和正己烷混合溶剂抽提得到自由态目标物,再通过碱性水解反应释放束缚态目标化合物。通过调节酸度（pH值）实现PBDEs和TBBPA的分离和提取。PBDEs由复合硅胶柱净化,运用气相色谱-质谱（负离子化学源）-分时段选择离子监测技术测定;TBBPA经重氮甲烷衍生化反应后由酸性硅胶柱预纯化,运用气相色谱-质谱（电子轰击源）-分时段选择离子监测技术测定。8种低溴联苯醚（BDE28,-47,-66,-100,-99,-154,-153,-183）,十溴联苯醚（BDE209）和TBBPA的检出限分别为0.6～12.5pg/g,172pg/g,4.2pg/g。方法具有良好的准确度和精确度,回收率均在74%～106%之间,RSD≤10%。对东江沉积物样品的分析表明,本方法能够实现不同形态的PBDEs和TBBPA的有效检测。

英文摘要：

An analysis method was developed for the determination of free and bound fractions of polybrominated ethers （PBDEs） and tetrabromobisphenol A （TBBPA） in sediment. The free PBDE and TBBPA were extracted with acetone/hexane （ 1 ： 1 ） mixed solvent, and the bound fraction was released from the sediment by saponification reaction at 80 ℃. PBDEs and TBBPA were separated via adjusting pH; PBDEs were determined by GC-negative chemical ionization （NCI）-MS after cleaned up by multilayer silica column, and TBB- PA was derivative before pre-separated by acid silica column and finally determined by GC-EI-MS. All of the target compounds were quantitative by internal standard method. The limits of detection of eight low brominated congeners （BDE28, -47, -66, -100, -99, -154, -153 and -183） , deca-BDE （BDE209）, and TBBPA were 0.6 -12.5 pg/g, 172 pg/g and 4.2 pg/g,respectively; This method is reliable and stable. The recoveries of all compounds were ranged from 74% to 106% and the relative standard deviations were below 10%. This method is suitable for the measurement of different forms of PBDEs and TBBPA in sediment under reliable quality assurance and quality control.