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引用本文:   相雷雷, 宋洋, 卞永荣, 生弘杰, 柳广霞, 蒋新, 李国华, 王芳. 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. 分析化学, 2016, 44(5): 671-677. doi:  10.11895/j.issn.0253-3820.150821 [复制]

Citation:   XIANG Lei-Lei , SONG Yang , BIAN Yong-Rong , SHENG Hong-Jie , LIU Guang-Xia , JIANG Xin , LI Guo-Hua , WANG Fang . A Purification Method for Determination of 10 Polybrominated Diphenyl Ethers in Soil Using Accelerated Solvent Extraction-Solid Phase Extraction. Chinese Journal of Analytical Chemistry, 2016, 44(5): 671-677. doi: 10.11895/j.issn.0253-3820.150821 [复制]

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

收稿日期: 2015-10-17

基金项目: 本文系江苏省自然科学基金杰出青年基金项目(No.BK20150050)、国家重点基础研究发展计划(973计划)项目(No.2014CB441105)、国家自然科学基金项目(Nos.21277148,41271464)和江苏省自然科学基金项目(No.BK20131463)资助

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

Received Date:  2015-10-17

Fund Project:  This work was supported by the Natural Science Fundation of Jiangsu Province for Distinguished Young Scholars (No. BK20150050), the Major State Basic Research Development Program of China (No. 2014CB441105), the National Natural Science Foundation of China (Nos. 21277148, 41271464) and the Natural Science Foundation of Jiangsu Province (No. BK20131463)

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/mL。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。

关键词:   土壤, 多溴联苯醚, 加速溶剂萃取, 固相萃取净化, 气相色谱
Key words:   Soil, Polybrominated diphenyl ethers, Accelerated solvent extraction, Solid phase extraction, Gas chromatography
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目录

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

相雷雷, 宋洋, 卞永荣, 生弘杰, 柳广霞, 蒋新, 李国华, 王芳

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