梁秀美, 夏海涛, 张维一, 林定鹏, 何如意, 郭秀珠, 陈官菊, 张井. 气相色谱-串联质谱法同时测定鲫鱼及产地底泥中41种清塘常用农药残留[J]. 农药学学报, 2023, 25(4): 915-929. DOI: 10.16801/j.issn.1008-7303.2023.0040
    引用本文: 梁秀美, 夏海涛, 张维一, 林定鹏, 何如意, 郭秀珠, 陈官菊, 张井. 气相色谱-串联质谱法同时测定鲫鱼及产地底泥中41种清塘常用农药残留[J]. 农药学学报, 2023, 25(4): 915-929. DOI: 10.16801/j.issn.1008-7303.2023.0040
    LIANG Xiumei, XIA Haitao, ZHANG Weiyi, LIN Dingpeng, HE Ruyi, GUO Xiuzhu, CHEN Guanju, ZHANG Jing. Determination of 41 pond cleaning commonly used pesticide residues in crucian carp and bottom sediment by gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2023, 25(4): 915-929. DOI: 10.16801/j.issn.1008-7303.2023.0040
    Citation: LIANG Xiumei, XIA Haitao, ZHANG Weiyi, LIN Dingpeng, HE Ruyi, GUO Xiuzhu, CHEN Guanju, ZHANG Jing. Determination of 41 pond cleaning commonly used pesticide residues in crucian carp and bottom sediment by gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2023, 25(4): 915-929. DOI: 10.16801/j.issn.1008-7303.2023.0040

    气相色谱-串联质谱法同时测定鲫鱼及产地底泥中41种清塘常用农药残留

    Determination of 41 pond cleaning commonly used pesticide residues in crucian carp and bottom sediment by gas chromatography-tandem mass spectrometry

    • 摘要: 采用改良QuEChERS前处理方法,结合气相色谱-串联质谱 (GC-MS/MS) 仪,建立了鲫鱼和产地底泥中41种农药残留的检测方法。鲫鱼样品用V (乙腈) : V (乙酸乙酯) = 1 : 1提取,经600 mg碱性氧化铝净化;产地底泥样品用乙酸乙酯提取,经600 mg弗罗里硅土和150 mg石墨化碳黑净化。用GC-MS/MS分析,采用HP-5MS柱进行分离,电子轰击离子源 (EI) 动态多反应监测模式 (dMRM) 检测,以空白基质匹配标准溶液外标法绘制标准曲线,进行定量。结果表明:1) 鲫鱼中41种农药的仪器检出限 (LOD) 在0.05~2.5 μg/L之间,方法定量限(LOQ)在0.1~5.0 μg/kg之间,线性相关系数 (r) 在0.9960~0.9999之间;在LOQ、2 LOQ 和10 LOQ 3个添加水平下,41种农药在鲫鱼中的平均回收率在73%~116%之间,相对标准偏差 (RSD) 在0.65%~13%之间 (n = 6)。2) 养殖底泥中41种农药的仪器LOD在0.05~2.5 μg/L之间,方法LOQ在0.1~5.0 μg/kg之间,r在0.9964~1.000之间;在LOQ、2 LOQ 和10 LOQ 3个添加水平下,41种农药在底泥中的平均回收率在73%~104%之间,RSD在0.051%~10%之间 (n = 6)。该方法前处理快速,检测方法灵敏、准确,在鲫鱼和底泥中检测酰胺类、三嗪类、苯基吡唑类、有机氯和有机磷等农药多残留具有较好的应用前景。

       

      Abstract: An analytical method for the determination of 41 pesticide residues in crucian carp and bottom sediment was established using modified QuEChERS sample preparation and gas chromatography-tandem mass spectrometry (GC-MS/MS). The crucian carp samples were extracted by acetonitrile and ethyl acetate (V:V = 1:1) and cleaned-up with 600 mg Alumina-B. The bottom sediment samples were extracted by ethyl acetate and cleaned-up with 600 mg Florisil and 150 mg Graphitized carbon black. The pesticide residues were analyzed by GC-MS/MS. A HP-5MS column was used for the separation, and the electron ionization (EI) was employed using dynamic multiple reaction monitoring (dMRM) mode for the detection. The matrix-matched external standard calibration curves were used for quantitative analysis. The method validation results indicated that in crucian carp, the instrumental limits of detection (LOD) for 41 pesticides were 0.05-2.5 μg/L, and the limits of quantification (LOQ) were 0.1-5.0 μg/kg for the method. The linear correlation coefficients (r) of the calibration curves were 0.9960-0.9999. The average recoveries at three spiked levels (LOQ, 2LOQ and 10LOQ) were 73%-116% (n = 6) with relative standard deviations (RSDs) of 0.65%-13%. In aquaculture sediment, the instrumental LODs for 41 pesticides were 0.05-2.5 μg/L, and the LOQs were 0.1-5.0 μg/kg for the method. r of the calibration curves were 0.9964-1.000. The average recoveries at three spiked levels (LOQ, 2LOQ and 10LOQ) were 73%-104% (n = 6) with RSDs of 0.051%-10%. The method was rapid, sensitive and accurate, and has a good application prospect in the detection of amides, triazines, phenyl pyrazoles, organochlorine and organophosphorus pesticide residues in crucian carp and bottom sediment.

       

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