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磁性分散固相萃取-QuEChERS结合气相色谱-串联质谱法检测不同柑橘基质中多种农药残留
引用本文:杨秦,张耀海,周杰,焦必宁.磁性分散固相萃取-QuEChERS结合气相色谱-串联质谱法检测不同柑橘基质中多种农药残留[J].农药学学报,2021,23(2):395-404.
作者姓名:杨秦  张耀海  周杰  焦必宁
作者单位:中国农业科学院/西南大学 柑桔研究所,农业农村部柑桔产品质量安全风险评估实验室(重庆),重庆 400712
基金项目:国家重点研发计划 (2019YFC1605604);现代农业 (柑橘) 产业技术体系 (CARS-26):国家农产品质量安全风险评估重大专项 (GJFP2019012)
摘    要:基于磁性分散固相萃取(MDSPE)-QuEChERS前处理技术,采用气相色谱-串联质谱法(GC-MS/MS)进行定性定量分析,建立了快速检测宽皮柑橘、甜橙、柠檬、柚子和金桔5种柑橘基质中75种农药残留的方法,优化了石墨化碳黑(GCB)、N-丙基乙二胺(PSA)和磁性纳米粒子(MNPS)用量对不同柑橘中目标分析物回收率的...

关 键 词:磁性分散固相萃取  QuEChERS  气相色谱-串联质谱  柑橘  农药多残留
收稿时间:2020-08-19

Analysis of multiple pesticide residues in different citrus matrices by magnetic dispersive solid phase extraction-QuEChERS combined with gas chromatography-tandem mass spectrometry
Institution:1.Laboratory of Risk Assessment for Citrus Quality and Safety, Ministry of Agriculture and Rural Affairs/Citrus Research Institute, Southwest University, Chinese Academy of Agricultural Sciences, Chongqing 400712, China2.Quality Supervision and Testing Center for Citrus and Seedling, Ministry of Agriculture and Rural Affairs, Chongqing 400712, China
Abstract:In this study, a rapid multi-residue detection method for 75 pesticide residues in 5 citrus, including mandarin, orange, lemon, pummelo and kumquat, was developed. Pesticide residues were extracted from citrus by magnetic dispersive solid phase extraction (MDSPE)-QuEChERS pretreatment and analyzed by gas chromatography-tandem mass spectrometry(GC-MS/MS). Graphitized carbon black (GCB), primary secondary amine (PSA) and magnetic nanoparticles (MNPS) were used as adsorbents in the (MDSPE)-QuEChERS pretreatment. In order to obtain the optimum recovery rate of pesticide analysis, the amounts of the adsorbents were investigated. Under the optimized conditions, a simple, fast, safe, cheap, reproducible, and applicable multi-residue method was established. Acceptable linearity was maintained at the concentration of 0.01 to 0.5 mg/kg, the average recoveries were in the range of 63% to 118%, and the relative standard deviations (RSDs) ranged from 0.30% to 16%. Also, the limits of detection (LODs) ranged from 1 to 7 μg/kg and the limits of quantification (LOQs) were in the range of 10-20 μg/kg.
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