| SHI Lei,SUN Yan-yan,SHEN Xiao-ming,LÜ Ai-juan,CAI Xiao-hu,LIU Jiao,SHEN Jia-lin.Determination of 24 Organochlorine Pesticides and Pyrethroids in Complex Matrix Soils by Comprehensive Two-dimensional Gas Chromatography with Micro-electron Capture Detector[J].Rock and Mineral Analysis,2020,39(6):856-865 |
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| Determination of 24 Organochlorine Pesticides and Pyrethroids in Complex Matrix Soils by Comprehensive Two-dimensional Gas Chromatography with Micro-electron Capture Detector |
| Received:June 09, 2019 Revised:September 30, 2019 |
| DOI：10.15898/j.cnki.11-2131/td.201906090082 |
| Key words: comprehensive two dimensional gas chromatography|Soxhlet's extraction|organochlorine pesticides|pyrethroids|soils |
| Author Name | Affiliation | | SHI Lei | Nanjing Center of Geological Survey, China Geological Survey, Nanjing 210016, China | | SUN Yan-yan | Nanjing Center of Geological Survey, China Geological Survey, Nanjing 210016, China | | SHEN Xiao-ming | Nanjing Center of Geological Survey, China Geological Survey, Nanjing 210016, China | | LÜ Ai-juan | Nanjing Center of Geological Survey, China Geological Survey, Nanjing 210016, China | | CAI Xiao-hu | Nanjing Center of Geological Survey, China Geological Survey, Nanjing 210016, China | | LIU Jiao | Nanjing Center of Geological Survey, China Geological Survey, Nanjing 210016, China | | SHEN Jia-lin | Nanjing Center of Geological Survey, China Geological Survey, Nanjing 210016, China |
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| Abstract: |
BACKGROUND: Currently the analysis methods of organochlorine pesticides and pyrethroids in environment samples are gas chromatography and gas chromatography-mass spectrometry (GC-MS). Gas chromatography with electron capture detector has been widely used in the study of environmental behavior of pollutants due to its high sensitivity. GC-MS has good qualitative results, but the detection sensitivity is relatively low.
OBJECTIVES: To establish an easy, highly efficient and precise method for determination of 20 organochlorine pesticides and 4 pyrethroids in complicated matrix soils.
METHODS: The residues of organochlorine pesticides and pyrethroids in samples from Jiangsu Province in 2018 were studied. In order to improve the qualitative accuracy and ensure the detection sensitivity, a comprehensive two-dimensional gas chromatography-electron capture detector detection method for determination of 20 organochlorine pesticides and 4 pyrethroids in complex-matrix soils was established. TG-35MS column (30m×0.25mm×0.25μm) was chosen as the column for the first dimension, and a DB-1 column (0.8m×0.18mm×0.18μm) was chosen as the column for the second dimension. The fresh sample was mixed with anhydrous sodium sulfate and extracted with hexane-acetone (1:1,V/V), subsequently purified by activated sheet copper. The analysis was conducted by GC×GC-μECD, qualified by retention time and quantified by external standard.
RESULTS: The proposed method showed good linearity with correlation coefficients (r) higher than 0.995 in the concentration range of 1.0-500μg/L, with the detection limits of 0.02-0.17μg/kg. The recovery of standard addition method ranged from 80.7% to 103.5%, and the relative standard deviations (n=6) were 1.84%-10.12%.
CONCLUSIONS: The proposed method combined high sensitivity detector with comprehensive two-dimension gas chromatography overcomes the matrix interference in complex sample, which shows a good detection sensitivity and peak capacity. The detection limit of the method is far lower than that of HJ 835-2017 standard (0.02-0.09). This method can provide reference for the analysis of multiple organochlorine pesticides and pyrethroids in complex-matrix soil. |
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