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

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: 6 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)

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.
- Soil,
- Polybrominated diphenyl ethers,
- Accelerated solvent extraction,
- Solid phase extraction,
- Gas chromatography
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