土壤中10种多溴联苯醚的加速溶剂-固相萃取净化方法优化研究

A Purification Method for Determination of 10 Polybrominated Diphenyl Ethers in Soil Using Accelerated Solvent Extraction-Solid Phase Extraction

建立了土壤中10种多溴联苯醚（PBDEs）的加速溶剂萃取-固相萃取净化-气相色谱分析测定方法。采用加速溶剂萃取（ASE）技术对土壤中10种PBDEs进行提取,并对4种萃取体系（正己烷、正己烷-丙酮（4∶1,V/V）、正己烷-丙酮（1∶1,V/V）、正己烷-二氯甲烷（1∶1,V/V））进行优化;采用固相萃取（SPE）技术对样品进行净化,制备了10种不同填料的SPE柱,通过洗脱实验和加标回收率实验对各SPE柱的净化性能进行对比筛选。最终优化条件为正己烷-丙酮（4∶1,V/V）体系提取,酸性硅胶柱净化。在优化条件下,10种PBDEs的回收率为74.4%~125.2%,相对标准偏差为4.4%~14.4%,方法检出限为0.04~0.22 ng/m L。本方法简单、快速、净化效果较好、重现性和回收率良好,可用于土壤样品中PBDEs的分析。

A method was established for the determination of 10 polybrominated diphenyl ethers （PBDEs） in soil using accelerated solvent extraction （ASE）, solid phase extraction （SPE） and gas chromatography with electron capture detector （GC-ECD）. ASE was used to obtain 10 PBDEs in soil and a good extraction system was investigated by comparison of kinds of extraction systems （n-hexane, n-hexane ： acetone （4： 1, V/V） , n-hexane ： acetone （1： 1, V/V） , and n-hexane ： dichloromethane （ 1 ： 1, V/V） ）. Besides, 10 kinds of SPE columns with different filters were applied to the purification of 10 PBDEs in soil solution. The optimized conditions were acquired by using the mixture of n-hexane and acetone （4： 1, V/V） as extract and acidic silica gel column for the purification. Under the optimized conditions, the average recoveries of 10 PBDEs in soil ranged from 74.4% to 125.2% with the RSDs of 4.4% - 14.4%. Method detection limits （MDLs） were 0.04-0.22 ng/mL. The method is simple, rapid and efficient, which has been successfully applied to determine 10 PBDEs in contaminated soil.