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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