超声波辅助萃取测定土壤中的多溴联苯醚

Ultrasound enhanced solvent extraction and GC-ECD for measurement of PBDEs in soil

对土壤中多溴联苯醚（PBDEs）的测定方法进行了研究。土壤样品经超声波辅助萃取后用硅胶氧化铝复合柱净化,再用带电子捕获检测器的气相色谱仪（GC-ECD）进行测定。该方法测定PBDEs各单体的相关系数（R^2）为0.999 54～0.999 97,方法线性关系良好。基质加标空白回收率在74.9%～118.1%,相对标准偏差（RSD）为5.9%～8.9%,方法检测限为5.9～9.2 ng/kg。

A fast and cost effective method for measuring concentrations of polybrominated diphenyl ethers （PBDEs） in soil was developed, The method featured a 10-minute ultrasound treatment of the solvent-soil mixture to improve the extraction efficiency. After series of clean-up, phase transfer and concentration steps,extracted PBDEs in the solvent phase were transferred to the 1 mL sample for analysis by GC-ECD, Using this method,excellent linear corre- lations were established for 7 PBDEs in the BDE-CSM standard with determination limits ranged from 5. 9 to 9.2 ng/kg. Recovery of those PBDEs spiked in 5 blanks ranged from 74.9% to 118.1% with a relative standard deviation between 5.9% and 8.9%. The method was successfully employed for measurement of PBDEs in 3 soil samples; the concentrations for the 7 PBDEs （0. 067～8. 900 ng/g） were in close agreement with those measured by the much more costly GC/MS method.