Innovation Center of Pesticide Research, Department of Applied Chemistry, College of Science, China Agricultural University, 2 Yuanmingyuan Western Road, Haidian District, Beijing, 100193, China.
Institute of Quality Standard and Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing, 100193, China.
Anal Bioanal Chem. 2024 Jan;416(3):663-674. doi: 10.1007/s00216-023-04542-9. Epub 2023 Jan 25.
Glufosinate is widely used to control various weeds. Glufosinate and its main metabolites have become the focus of attention because of their high water solubility and persistence in aquatic systems. Quantification of the agrochemical product and its metabolite residues is essential for the safety of agricultural products. In this study, a highly specific, simple method was developed to directly determine glufosinate and its metabolite residues in 21 plant origin foods by liquid chromatography with tandem mass spectrometry (LC-MS/MS), and it was validated on 11 foods in five laboratories. Finally, the repeatability limit, reproducibility limit, and uncertainty of the method were calculated based on these validated data and used to support the more accurate detection results. Four different chromatographic columns were used to analyze three target compounds, and the anionic polar pesticide column showed the optimum separation and peak shape. Composition of the mobile phase, extraction solvent, and the clean-up procedure were optimized. The developed method was validated on 21 plant origin foods. The average recoveries were 74-115% for all matrices. The validation results of five laboratories showed this method had a good repeatability (RSD < 9.5%) and reproducibility (RSD < 18.9%). The method validation parameters met the requirements of guidance established by the European Union (EU) and China for pesticide residue analysis. This methodology can be used for a routine monitoring that performs well for glufosinate and its metabolite residues.
草铵膦被广泛用于控制各种杂草。由于其在水生系统中具有高水溶性和持久性,草铵膦及其主要代谢物已成为关注焦点。对农用化学品及其代谢物残留的定量分析对于农产品的安全至关重要。在本研究中,开发了一种通过液相色谱-串联质谱(LC-MS/MS)直接测定 21 种植物源食品中草铵膦及其代谢物残留的高度特异性、简单方法,并在五个实验室的 11 种食品上进行了验证。最后,根据这些验证数据计算方法的重复性限、再现性限和不确定度,并用于支持更准确的检测结果。使用了四种不同的色谱柱来分析三种目标化合物,阴离子极性农药柱显示出最佳的分离和峰形。优化了流动相组成、提取溶剂和净化程序。开发的方法在 21 种植物源食品上进行了验证。所有基质的平均回收率均为 74-115%。五个实验室的验证结果表明,该方法具有良好的重复性(RSD<9.5%)和再现性(RSD<18.9%)。方法验证参数符合欧盟(EU)和中国制定的农药残留分析指南的要求。该方法可用于常规监测,对草铵膦及其代谢物残留具有良好的监测效果。