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Detection of 9 kinds of carbamate pesticides in Vigna unguiculata by magnetic covalent organic framework-based solid phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry
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Ying-Qi XU1, 2, 3, #, Tong LIU2, 3, #, Xiu-Li XU2, 3, Xiu-Juan WANG2, 3, Jian HE4, Meng HU5, Xiao-Yan PEI4, Qing-Li YANG1, Xiu-Dan HOU1, *, Feng ZHANG2, 3, *
Journal of Food Safety & Quality | 2025, 16(13) : 77 - 86
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Journal of Food Safety & Quality | 2025, 16(13): 77-86
• Highlight: Analysis and Monitoring of Toxic and Harmful Substances in Food •
Detection of 9 kinds of carbamate pesticides in Vigna unguiculata by magnetic covalent organic framework-based solid phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry
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Ying-Qi XU1, 2, 3, #, Tong LIU2, 3, #, Xiu-Li XU2, 3, Xiu-Juan WANG2, 3, Jian HE4, Meng HU5, Xiao-Yan PEI4, Qing-Li YANG1, Xiu-Dan HOU1, *, Feng ZHANG2, 3, *
Affiliations
  • 1 School of Food Science and Engineering, Qingdao Agricultural University, Qingdao 266109, China
  • 2 Institute of Food Safety, Chinese Academy of Quality and Inspection & Testing, Beijing 100176, China
  • 3 Key Laboratory of Food Quality and Safety, State Administration for Market Regulation, Beijing 100176, China
  • 4 National Dairy Technology Innovation Center, Hohhot 010010, China
  • 5 Yili Group, Hohhot 010010, China
Published: 2025-07-15 doi: 10.19812/j.cnki.jfsq11-5956/ts.20250412003
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Objective To establish a magnetic solid phase extraction (MSPE) approach based on covalent organic framework materials in combination with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for the efficient determination of 9 kinds of carbamate pesticides (CPs) in Vigna unguiculata. Methods After the extraction of Vigna unguiculata samples, the novel Fe3O4@TAPOB-BDTB material was employed for magnetic solid-phase extraction and purification. After filtration, the samples were separated by a C18 chromatographic column and quantitatively analyzed using multiple reaction monitoring in the electrospray positive ion mode. Results The established analytical methods for the 9 kinds of CPs exhibited excellent linearity within the concentration range of 0.02-100.00 μg/kg, with the determination coefficients (r2) all exceeding 0.9989. The spiked recovery rates were within the range of 80.33%-108.63%, and both the intra-day and inter-day precisions were less than 8.89%. The detection limits of the methods were 0.005-0.010 μg/kg, and the limits of quantitation were 0.02 μg/kg, which were significantly below the maximum residue limits specified in GB 2763—2021 National food safety standard-Maximum residue limits of pesticides in food and EU Regulation No 396/2005, ensuring compliance within an academic context. Conclusion The covalent organic framework materials synthesize in this study demonstrate exceptional adsorption capacity for CPs via π-π interactions and hydrogen bonding. Furthermore, the develope MSPE-HPLC-MS/MS method enables rapid, highly sensitive, and precise detection of CPs in Vigna unguiculata, thereby offering an efficient and innovative approach for monitoring pesticide residues in agricultural products.

covalent organic framework materials  /  high performance liquid chromatography-tandem mass spectrometry  /  carbamate pesticides  /  magnetic solid phase extraction
Ying-Qi XU, Tong LIU, Xiu-Li XU, Xiu-Juan WANG, Jian HE, Meng HU, Xiao-Yan PEI, Qing-Li YANG, Xiu-Dan HOU, Feng ZHANG. Detection of 9 kinds of carbamate pesticides in Vigna unguiculata by magnetic covalent organic framework-based solid phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety & Quality, 2025 , 16 (13) : 77 -86 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250412003
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Article Info
doi: 10.19812/j.cnki.jfsq11-5956/ts.20250412003
  • Receive Date：2025-04-12
  • Online Date：2026-01-12
  • Published：2025-07-15
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  • Received：2025-04-12
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Affiliations
    1 School of Food Science and Engineering, Qingdao Agricultural University, Qingdao 266109, China
    2 Institute of Food Safety, Chinese Academy of Quality and Inspection & Testing, Beijing 100176, China
    3 Key Laboratory of Food Quality and Safety, State Administration for Market Regulation, Beijing 100176, China
    4 National Dairy Technology Innovation Center, Hohhot 010010, China
    5 Yili Group, Hohhot 010010, China
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表12种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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