Citation: WU Jing, HU Ji-Cheng, MA Yu-Long, WANG Shi-Jie, WANG Ying, JIN Jun. Determination of Dioxin-like Compounds in Soil by Accelerated Solvent Extraction-Silica Gel Column Cleanup-Basic Alumina Column Separation Coupled with Gas Chromatography-Triple Quadrupole Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2017, 45(6): 799-808. doi: 10.11895/j.issn.0253-3820.170017 shu

Determination of Dioxin-like Compounds in Soil by Accelerated Solvent Extraction-Silica Gel Column Cleanup-Basic Alumina Column Separation Coupled with Gas Chromatography-Triple Quadrupole Mass Spectrometry

WU Jing ^1, ,
HU Ji-Cheng ^1,2 ,
MA Yu-Long ¹ ,
WANG Shi-Jie ¹ ,
WANG Ying ^1,2 ,
JIN Jun ^1,2

1.
College of Life and Environment Sciences, Minzu University of China, Beijing 100081, China;
2.
Engineering Research Center of Food Environment and Public Health, Beijing 100081, China

Received Date: 10 January 2017
Revised Date: 5 April 2017

Fund Project: This work was supported by the National Natural Science Foundation of China (No. 21407185), the Fundamental Research Funds for the Central Universities (Nos. 2017MDYL31, 2015MDTD23C), the Institution of Higher Education Innovation Talent Recruitment Program (No. B08044), and the National College Students' Innovative Training Program (No. GCCX2016110042).

A method for determination of PCDD/Fs, PCBs and PCNs in soil sample was developed by using accelerated solvent extraction (ASE)-silica gel column cleanup-basic alumina column separation coupled with GC-MS/MS. The sample was extracted by ASE with Hexane-methylene chloride (Hex-DCM, 50:50, V/V) at 120℃. The basic alumina column was used to separate PCDD/Fs, PCBs and PCNs. The extracts were eluted with Hex-DCM (95:5, V/V) to obtain PCBs and PCNs, followed by Hex-DCM (50:50, V/V) to obtain PCDD/Fs. The limits of detection (LOD) were in the range of 0.04-0.25 μg/L, 0.10-0.20 μg/L and 0.01-0.05 μg/L for PCDD/Fs, PCBs, PCNs, respectively. The relative standard deviations (RSDs) of average relative response factors (RRF) were below 13%. The recoveries of ¹³C-labeled internal standards of the three classes of analytes were 50%-95%, 51%-103% and 49%-74%, respectively. Concentrations of ∑PCDD/Fs, ∑PCBs and ∑PCNs in soil samples were 16.1-1148 pg/g, 6.6-152.6 pg/g and 10.9-99.5 pg/g, respectively. The results were consistent with that of high resolution mass spectrometery
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