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 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

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

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。方法 豇豆样品提取后采用新型Fe3O4@TAPOB-BDTB材料进行MSPE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0.02~100.00 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等于8.89%。方法检出限为0.005~0.010 μg/kg, 定量限为0.02 μg/kg, 显著低于GB 2763—2021《食品安全国家标准 食品中农药最大残留限量》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 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.