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 |
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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. |
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作者姓名: | 杨秦 张耀海 周杰 焦必宁 |
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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 |
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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) |
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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...
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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 |
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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 |
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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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