Determination of 24 Organochlorine Pesticides and Pyrethroids in Complex Matrix Soils by Comprehensive Two-dimensional Gas Chromatography with Micro-electron Capture Detector

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 poll...

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Main Authors: SHI Lei, SUN Yan-yan, SHEN Xiao-ming, LÜ Ai-juan, CAI Xiao-hu, LIU Jiao, SHEN Jia-lin
Format: Article
Language:English
Published: Science Press, PR China 2020-11-01
Series:Yankuang ceshi
Subjects:
Online Access:http://www.ykcs.ac.cn/en/article/doi/10.15898/j.cnki.11-2131/td.201906090082
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author SHI Lei
SUN Yan-yan
SHEN Xiao-ming
LÜ Ai-juan
CAI Xiao-hu
LIU Jiao
SHEN Jia-lin
author_facet SHI Lei
SUN Yan-yan
SHEN Xiao-ming
LÜ Ai-juan
CAI Xiao-hu
LIU Jiao
SHEN Jia-lin
author_sort SHI Lei
collection DOAJ
description 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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spelling doaj.art-16b255521a1945bca346ad48e790db212023-01-13T09:16:34ZengScience Press, PR ChinaYankuang ceshi0254-53572020-11-0139685686510.15898/j.cnki.11-2131/td.201906090082yk201906090082Determination of 24 Organochlorine Pesticides and Pyrethroids in Complex Matrix Soils by Comprehensive Two-dimensional Gas Chromatography with Micro-electron Capture DetectorSHI Lei0SUN Yan-yan1SHEN Xiao-ming2LÜ Ai-juan3CAI Xiao-hu4LIU Jiao5SHEN Jia-lin6Nanjing Center of Geological Survey, China Geological Survey, Nanjing 210016, ChinaNanjing Center of Geological Survey, China Geological Survey, Nanjing 210016, ChinaNanjing Center of Geological Survey, China Geological Survey, Nanjing 210016, ChinaNanjing Center of Geological Survey, China Geological Survey, Nanjing 210016, ChinaNanjing Center of Geological Survey, China Geological Survey, Nanjing 210016, ChinaNanjing Center of Geological Survey, China Geological Survey, Nanjing 210016, ChinaNanjing Center of Geological Survey, China Geological Survey, Nanjing 210016, ChinaBACKGROUND 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.http://www.ykcs.ac.cn/en/article/doi/10.15898/j.cnki.11-2131/td.201906090082comprehensive two dimensional gas chromatographysoxhlet's extractionorganochlorine pesticidespyrethroidssoils
spellingShingle 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
Yankuang ceshi
comprehensive two dimensional gas chromatography
soxhlet's extraction
organochlorine pesticides
pyrethroids
soils
title Determination of 24 Organochlorine Pesticides and Pyrethroids in Complex Matrix Soils by Comprehensive Two-dimensional Gas Chromatography with Micro-electron Capture Detector
title_full Determination of 24 Organochlorine Pesticides and Pyrethroids in Complex Matrix Soils by Comprehensive Two-dimensional Gas Chromatography with Micro-electron Capture Detector
title_fullStr Determination of 24 Organochlorine Pesticides and Pyrethroids in Complex Matrix Soils by Comprehensive Two-dimensional Gas Chromatography with Micro-electron Capture Detector
title_full_unstemmed Determination of 24 Organochlorine Pesticides and Pyrethroids in Complex Matrix Soils by Comprehensive Two-dimensional Gas Chromatography with Micro-electron Capture Detector
title_short Determination of 24 Organochlorine Pesticides and Pyrethroids in Complex Matrix Soils by Comprehensive Two-dimensional Gas Chromatography with Micro-electron Capture Detector
title_sort determination of 24 organochlorine pesticides and pyrethroids in complex matrix soils by comprehensive two dimensional gas chromatography with micro electron capture detector
topic comprehensive two dimensional gas chromatography
soxhlet's extraction
organochlorine pesticides
pyrethroids
soils
url http://www.ykcs.ac.cn/en/article/doi/10.15898/j.cnki.11-2131/td.201906090082
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