Simultaneous determination of triazine herbicides and their metabolites in shellfish by HPLC-MS/MS combined with Q/E-Orbitrap HRMS

Triazine herbicides are used extensively in agriculture and aquaculture worldwide because of their broad effectiveness in weed control. However, after they are discharged into the sea, they seriously contaminate aquatic ecosystems and threaten aquatic organisms, especially shellfish. Currently, ther...

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Veröffentlicht in:Analytical and bioanalytical chemistry 2021-10, Vol.413 (25), p.6239-6252
Hauptverfasser: Sun, Xiaojie, Gao, Jinfang, Xing, Jun, Xing, Lihong, Guo, Mengmeng, Peng, Jixing, Li, Zhaoxin, Tan, Zhijun
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container_end_page 6252
container_issue 25
container_start_page 6239
container_title Analytical and bioanalytical chemistry
container_volume 413
creator Sun, Xiaojie
Gao, Jinfang
Xing, Jun
Xing, Lihong
Guo, Mengmeng
Peng, Jixing
Li, Zhaoxin
Tan, Zhijun
description Triazine herbicides are used extensively in agriculture and aquaculture worldwide because of their broad effectiveness in weed control. However, after they are discharged into the sea, they seriously contaminate aquatic ecosystems and threaten aquatic organisms, especially shellfish. Currently, there are no established methods for the detection and confirmation of triazine herbicides and their metabolites in biological matrixes. Hence, the food safety of aquatic products cannot be accurately evaluated, which creates a technical barrier against international aquatic product trade. In this study, for the first time, a method was developed for the analysis and confirmation of seven triazine herbicides and 13 metabolites in shellfish, based on alkaline acetonitrile extraction and neutral Al 2 O 3 cartridge purification coupled with internal standard calibration. Specifically, quantitative and qualitative analysis was conducted using high-performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS), and accurate identification was carried out by quadrupole orbitrap high-resolution mass spectrometry (Q/E Orbitrap HRMS). The results showed that target analytes demonstrated good linearity within the corresponding range ( R 2 > 0.995). The limit of detection and limit of quantitation of the proposed method were 0.1 and 0.3 μg/kg, respectively. The average recoveries of analytes were between 70.0% and 120% when spiked at three levels with blank oyster ( Crassostrea gigas ) as the matrix, and the relative standard deviations (RSDs) were all less than 12% ( n =6). The proposed method was successfully applied for the detection of triazine herbicide residues in oyster samples during actual breeding, and the presence of DIP, HP, DEHA, and other metabolites in positive samples was confirmed by Q/E Orbitrap HRMS. This method exhibits high accuracy, high sensitivity, and good reproducibility. It has promising application prospects in the field of hazard analysis and the positive identification of aquatic products. Graphical abstract
doi_str_mv 10.1007/s00216-021-03579-y
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However, after they are discharged into the sea, they seriously contaminate aquatic ecosystems and threaten aquatic organisms, especially shellfish. Currently, there are no established methods for the detection and confirmation of triazine herbicides and their metabolites in biological matrixes. Hence, the food safety of aquatic products cannot be accurately evaluated, which creates a technical barrier against international aquatic product trade. In this study, for the first time, a method was developed for the analysis and confirmation of seven triazine herbicides and 13 metabolites in shellfish, based on alkaline acetonitrile extraction and neutral Al 2 O 3 cartridge purification coupled with internal standard calibration. Specifically, quantitative and qualitative analysis was conducted using high-performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS), and accurate identification was carried out by quadrupole orbitrap high-resolution mass spectrometry (Q/E Orbitrap HRMS). The results showed that target analytes demonstrated good linearity within the corresponding range ( R 2 &gt; 0.995). The limit of detection and limit of quantitation of the proposed method were 0.1 and 0.3 μg/kg, respectively. The average recoveries of analytes were between 70.0% and 120% when spiked at three levels with blank oyster ( Crassostrea gigas ) as the matrix, and the relative standard deviations (RSDs) were all less than 12% ( n =6). The proposed method was successfully applied for the detection of triazine herbicide residues in oyster samples during actual breeding, and the presence of DIP, HP, DEHA, and other metabolites in positive samples was confirmed by Q/E Orbitrap HRMS. This method exhibits high accuracy, high sensitivity, and good reproducibility. It has promising application prospects in the field of hazard analysis and the positive identification of aquatic products. 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However, after they are discharged into the sea, they seriously contaminate aquatic ecosystems and threaten aquatic organisms, especially shellfish. Currently, there are no established methods for the detection and confirmation of triazine herbicides and their metabolites in biological matrixes. Hence, the food safety of aquatic products cannot be accurately evaluated, which creates a technical barrier against international aquatic product trade. In this study, for the first time, a method was developed for the analysis and confirmation of seven triazine herbicides and 13 metabolites in shellfish, based on alkaline acetonitrile extraction and neutral Al 2 O 3 cartridge purification coupled with internal standard calibration. Specifically, quantitative and qualitative analysis was conducted using high-performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS), and accurate identification was carried out by quadrupole orbitrap high-resolution mass spectrometry (Q/E Orbitrap HRMS). The results showed that target analytes demonstrated good linearity within the corresponding range ( R 2 &gt; 0.995). The limit of detection and limit of quantitation of the proposed method were 0.1 and 0.3 μg/kg, respectively. The average recoveries of analytes were between 70.0% and 120% when spiked at three levels with blank oyster ( Crassostrea gigas ) as the matrix, and the relative standard deviations (RSDs) were all less than 12% ( n =6). The proposed method was successfully applied for the detection of triazine herbicide residues in oyster samples during actual breeding, and the presence of DIP, HP, DEHA, and other metabolites in positive samples was confirmed by Q/E Orbitrap HRMS. This method exhibits high accuracy, high sensitivity, and good reproducibility. It has promising application prospects in the field of hazard analysis and the positive identification of aquatic products. 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However, after they are discharged into the sea, they seriously contaminate aquatic ecosystems and threaten aquatic organisms, especially shellfish. Currently, there are no established methods for the detection and confirmation of triazine herbicides and their metabolites in biological matrixes. Hence, the food safety of aquatic products cannot be accurately evaluated, which creates a technical barrier against international aquatic product trade. In this study, for the first time, a method was developed for the analysis and confirmation of seven triazine herbicides and 13 metabolites in shellfish, based on alkaline acetonitrile extraction and neutral Al 2 O 3 cartridge purification coupled with internal standard calibration. Specifically, quantitative and qualitative analysis was conducted using high-performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS), and accurate identification was carried out by quadrupole orbitrap high-resolution mass spectrometry (Q/E Orbitrap HRMS). The results showed that target analytes demonstrated good linearity within the corresponding range ( R 2 &gt; 0.995). The limit of detection and limit of quantitation of the proposed method were 0.1 and 0.3 μg/kg, respectively. The average recoveries of analytes were between 70.0% and 120% when spiked at three levels with blank oyster ( Crassostrea gigas ) as the matrix, and the relative standard deviations (RSDs) were all less than 12% ( n =6). The proposed method was successfully applied for the detection of triazine herbicide residues in oyster samples during actual breeding, and the presence of DIP, HP, DEHA, and other metabolites in positive samples was confirmed by Q/E Orbitrap HRMS. This method exhibits high accuracy, high sensitivity, and good reproducibility. It has promising application prospects in the field of hazard analysis and the positive identification of aquatic products. Graphical abstract</abstract><cop>Berlin/Heidelberg</cop><pub>Springer Berlin Heidelberg</pub><pmid>34389879</pmid><doi>10.1007/s00216-021-03579-y</doi><tpages>14</tpages></addata></record>
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subjects Acetonitrile
Agrochemicals
Aluminum oxide
Analytical Chemistry
Animals
Aquaculture
Aquatic ecosystems
Aquatic organisms
Biochemistry
Characterization and Evaluation of Materials
Chemistry
Chemistry and Materials Science
Chromatography, High Pressure Liquid - methods
Food Contamination - analysis
Food safety
Food Science
Hazard assessment
Herbicide residues
Herbicides
Herbicides - chemistry
Herbicides - metabolism
High performance liquid chromatography
Identification and classification
Laboratory Medicine
Limit of Detection
Liquid chromatography
Mass spectrometry
Mass Spectrometry - methods
Mass spectroscopy
Metabolites
Methods
Monitoring/Environmental Analysis
Ostreidae - chemistry
Ostreidae - metabolism
Oysters
Pesticide Residues - chemistry
Product safety
Quadrupoles
Qualitative analysis
Quantitation
Reproducibility of Results
Research Paper
Scientific imaging
Shellfish
Shellfish - analysis
Spectroscopy
Triazine
Triazines - chemistry
Weed control
title Simultaneous determination of triazine herbicides and their metabolites in shellfish by HPLC-MS/MS combined with Q/E-Orbitrap HRMS
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