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| 磁性共价有机框架材料固相萃取结合高效液相色谱-串联质谱法检测豇豆中9种氨基甲酸酯类农药 |
| Detection of 9 Carbamate Pesticides in Cowpea by Magnetic Covalent Organic Framework-Based Solid Phase Extraction Coupled with High-Performance Liquid Chromatography-Tandem Mass Spectrometry |
| 投稿时间：2025-04-12 修订日期：2025-06-09 |
| DOI： |
| 中文关键词: 共价有机框架材料 高效液相色谱-串联质谱 氨基甲酸酯类农药 磁固相萃取 |
| 英文关键词:Covalent organic framework materials High-performance liquid chromatography-tandem mass spectrometry Carbamate pesticides Magnetic solid-phase extraction |
| 基金项目:检科院工作经费项目(2022-科研攻关-13)、国家乳业技术创新中心项目(2024-JSGG-016) |
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| 中文摘要: |
| 目的 建立基于新型磁性共价有机框架材料（Fe3O4@TAPOB-BDTB）的磁固相萃取（magnetic solid-phase extraction，MSPE）联用高效液相色谱-串联质谱（high performance liquid chromatography-tandem mass spectrometry，HPLC-MS/MS）技术，实现豇豆中9种氨基甲酸酯类农药（carbamate pesticides，CPs）残留的痕量检测。方法 豇豆样品提取后采用新型Fe3O4@TAPOB-BDTB材料进行磁固相萃取净化，经过滤后，通过C18色谱柱分离，采用电喷雾正离子模式进行多反应监测定量分析。结果 所建立的9种CPs分析方法在0.05～100 μg/kg浓度范围内线性良好，决定系数（r2）均大于0.9989。加标回收率为80.33%～108.63%，日内和日间精密度均小于8.89%。方法检出限为0.005～0.010 μg/kg，定量限为0.01～0.02 μg/kg，显著低于GB 2763—2021和欧盟No 396/2005法规最大残留限量要求。结论 本研究制备的共价有机框架材料通过π-π作用及氢键效应，对CPs表现出优异的吸附能力，所开发的MSPE-HPLC-MS/MS方法适用于豇豆中CPs的快速、高灵敏、准确检测，为农产品中农药残留的监控提供了一种高效的新手段。 |
| 英文摘要: |
| 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 cowpea. Methods After the extraction of cowpea 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 0.05-100 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 quantification limits were 0.01-0.05 μg/kg, which were significantly below the maximum residue limits specified in GB 2763—2021 and EU Regulation No 396/2005, ensuring compliance within an academic context. Conclusion The covalent organic framework materials synthesized in this study demonstrate exceptional adsorption capacity for CPs via π-π interactions and hydrogen bonding. Furthermore, the developed MSPE-HPLC-MS/MS method enables rapid, highly sensitive, and precise detection of CPs in cowpeas, thereby offering an efficient and innovative approach for monitoring pesticide residues in agricultural products. |
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