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. DOI: 10.16801/j.issn.1008-7303.2021.0056
    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. DOI: 10.16801/j.issn.1008-7303.2021.0056
    YANG Qin, ZHANG Yaohai, ZHOU Jie, JIAO Bining. Analysis of multiple pesticide residues in different citrus matrices by magnetic dispersive solid phase extraction-QuEChERS combined with gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2021, 23(2): 395-404. DOI: 10.16801/j.issn.1008-7303.2021.0056
    Citation: YANG Qin, ZHANG Yaohai, ZHOU Jie, JIAO Bining. Analysis of multiple pesticide residues in different citrus matrices by magnetic dispersive solid phase extraction-QuEChERS combined with gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2021, 23(2): 395-404. DOI: 10.16801/j.issn.1008-7303.2021.0056

    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

    Analysis of multiple pesticide residues in different citrus matrices by magnetic dispersive solid phase extraction-QuEChERS combined with gas chromatography-tandem mass spectrometry

    • 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影响。在优化条件下,目标分析物的线性范围在0.01~0.5 mg/kg之间,平均回收率为63%~118%,相对标准偏差为0.30%~16%。方法的检出限 (LOD) 为1~7 μg/kg,定量限 (LOQ) 为10~20 μg/kg。该方法简便、快速、安全、价格低廉,重现性良好,可用于不同柑橘中多种农药残留的快速确证检测。

       

      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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