Citation: WEI Dan, GUO Ming, WU Huizhen, ZHANG Ju. Determination of 16 polycyclic aromatic hydrocarbon and 23 organochlorine residues in soil by accelerated solvent extraction and magnetic solid phase purification- gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2020, 38(8): 945-952. doi: 10.3724/SP.J.1123.2019.12028 shu

Determination of 16 polycyclic aromatic hydrocarbon and 23 organochlorine residues in soil by accelerated solvent extraction and magnetic solid phase purification- gas chromatography-tandem mass spectrometry

WEI Dan ^1,, ,
GUO Ming ² ,
WU Huizhen ³ ,
ZHANG Ju ¹

1.
College of Bioscience and Engineering, Hebei University of Economics and Business;Shijiazhuang 050061, China;
2.
Center of Analysis and Testing, Zhejiang Research Institute of Chemical Industry Co., Ltd., Hangzhou 310023, China;
3.
College of Biological and Environmental Engineering, Zhejiang Shuren University, Hangzhou 310015, China

Corresponding author: WEI Dan, 1422547228@qq.com
Received Date: 20 December 2019

Fund Project: the Scientific Research Project of the Zhejiang Provincial Education Department (No. Y201840776)

A method combining accelerated solvent extraction (ASE) with magnetic solid-phase extraction (MSPE) and gas chromatography-mass spectrometry (GC-MS) was developed for the simultaneous detection of polycyclic aromatic hydrocarbon (PAH) and organochlorinepesticide (OCP) residues in soil samples. The analytes in the soil samples were extracted using an acetone/n-hexane (1:1, v/v) mixture for 5 min at 100℃. Then, the extraction pool was heated for 5 min under an extractive pressure of 11.032 MPa for three cycles. The extraction pool was washed with an acetone/n-hexane (1:1, v/v) mixture accounting for 60% of the pool volume, followed by nitrogen purging for 100 s. The extract was purified by MSPE using self-made magnetic ZIF-8/nZVI materials at room temperature. The analytes were detected by GC-MS/MS. Under the optimized conditions, good linearities were obtained for the 16 PAHs and the 23 OCPs in the range of 5-200 μg/kg, with correlation coefficients (r²) above 0.99. The limits of detection (LODs) were 0.04-1.21 μg/kg. At three spiked levels in the soil samples, the recoveries of the 39 analytes were between 63.9% and 112.1%, with relative standard deviations (RSDs) between 0.4% and 26.2%. The method was demonstrated to be successful for the determination of 16 PAH and 23 OCP residues in soil samples, with good recoveries.
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