Optimization and validation of an oxidation and solid-phase extraction procedure for analysis of imidacloprid and its metabolites in cereals using ultra-performance liquid chromatography tandem mass spectrometry
文献类型： 外文期刊
作者： Wang, Tan 1 ; Zhao, Yueliang 2 ; Zhang, Songhan 3 ; Ma, Lin 3 ; Sun, Qiang 1 ; Zhao, Li 3 ; Wang, Weimin 1 ; Dong, Maofeng 1 ;
作者机构： 1.Shanghai Acad Agr Sci, Inst Agrofood Stand & Testing Technol, Pesticide Safety Evaluat Res Ctr,Minist Agr & Rura, Key Lab Safety Assessment Environm Agr Genet Modif, Shanghai 201106, Peoples R China
2.Shanghai Ocean Univ, Coll Food Sci & Technol, Shanghai 201306, Peoples R China
3.Shanghai Agr Tech Extens Serv Ctr, Shanghai 201103, Peoples R China
4.Shanghai Acad Agr Sci, Pesticide Safety Evaluat Res Ctr, Shanghai 2011106, Peoples R China
关键词： Imidacloprid; 6-Chloronicotinic acid; Oxidation; UPLC-MS/MS; Cereals
期刊名称：FOOD CONTROL （ 影响因子：6.0； 五年影响因子：5.8 ）
ISSN： 0956-7135
年卷期： 2023 年 152 卷
页码：
收录情况： SCI
摘要： A simple and reliable ultraperformance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was proposed for analysis of the total residues of imidacloprid and its 6-chloropyridinyl metabolites in cereals. The method consisted of extraction with acidic acetonitrile, conversion of the analytes into 6-chloronicotinic acid by oxidation, cleanup with C18 cartridges, and UPLC-MS/MS detection. The validation results met the requirements of the guidelines for the detection of pesticide residues in EU and China, including the linearity (R-2 = 0.998), matrix effect (- 0.5 similar to-7.1%), accuracy (75.1-109.6%), precision (3.5-13.0%), metabolite conversion efficiency (81.6-102.3%), and sensitivity (limit of detection (LOD) of 0.0015 mg/kg and limit of quantification (LOQ) of 0.0050 mg/kg). The established method met the requirements of the residue definition and the maximum residue levels (MRLs) of imidacloprid in cereals, and was further applied to investigate the residues and dissipation of imidacloprid and its metabolites in wheat samples after field application.
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