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

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[J]. 分析化学, 2016, 44(5): 671-677. doi: 10.11895/j.issn.0253-3820.150821 shu

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[J]. Chinese Journal of Analytical Chemistry, 2016, 44(5): 671-677. doi: 10.11895/j.issn.0253-3820.150821 shu

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 ^1,2, ,
宋洋 ^2, ,
卞永荣 ^2, ,
生弘杰 ^2, ,
柳广霞 ^2, ,
蒋新 ^2, ,
李国华 ^1, ,
王芳 ^2,

1.
江苏省农药学重点实验室, 南京农业大学理学院, 南京 210095;
2.
土壤与农业可持续发展国家重点实验室, 中国科学院南京土壤研究所, 南京 210008
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

摘要: 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:

English

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

1.
Jiangsu Key Laboratory of Pesticide Science, College of Science, Nanjing Agricultural University, Nanjing 210095, China;
2.
State Key Laboratory of Soil and Sustainable Agriculture, Institute of Soil Science, Chinese Academy of Sciences, Nanjing, 210008, China
Received Date: 17 October 2015
Revised Date: 06 January 2016
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)

Abstract: 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.

Key words:

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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

English

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

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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

English

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

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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