【摘要】 建立了基质固相分散萃取-气相色谱/质谱法测定土壤中13种多溴联苯醚的分析方法.对固相分散剂种类、样品与分散剂用量比例、洗脱溶剂及用量进行了选择和优化.最佳前处理条件为:2g样品与4g酸性硅胶固相分散剂研磨10min,混合物装入预先填好4g无水硫酸钠和4g酸性硅胶的玻璃柱中,以50mL正己烷/二氯甲烷（v:v=1:1）混合液洗脱并浓缩至0.5 mL,进GC-MS分析.13种多溴联苯醚在2²00ng·g^-1内呈良好的线性关系（R2>0.992）.平均加标回收率在81%¹03%,相对标准偏差（RSD）小于15%（n=3）,方法检出限为75⁹50pg·g^-1,可以满足土壤中痕量多溴联苯醚残留分析的要求.更多还原

【Abstract】 A matrix solid phase dispersion extraction-gas chromatography/mass spectrometric method has been developed for the determination of 13 polybrominated diphenyl ethers in soil.Parameters including species of solid-phase dispersant,ratios of sample to dispersant,elution species and amount have been optimized.The best pretreatment conditions are as follows:2 g sample was mixed with 4 g acidic silica,and then grinded for 10 min.The mixture was loaded into a glass column pre-filled with 4 g anhydrous sodium sulfate and 4 g acidic silica.Hexane/dichloromethane（v:v=1:1,50mL）mixture was used as eluent.The elution was concentrated to 0.5 mL prior to GC/MS analysis.13 kinds of PBDEs all show good linear relationships（R2> 0.992）in the range from 2 to 200 ng·g^-1.The average recoveries are 81%to 103%and the relative standard deviation is less than 15%（n=3）.The method detection limits ranged from 75 to 950 pg·g^-1,which meets the need for the analysis of trace PBDEs in soil.更多还原