李春丽, 乐渊, 尹桂豪, 阳辛凤, 黎舒怀, 刘春华. 超高效液相色谱-串联质谱法测定莲雾中多菌灵、噻菌灵和甲霜灵残留[J]. 农药学学报, 2015, 17(5): 579-584. DOI: 10.3969/j.issn.1008-7303.2015.05.11
    引用本文: 李春丽, 乐渊, 尹桂豪, 阳辛凤, 黎舒怀, 刘春华. 超高效液相色谱-串联质谱法测定莲雾中多菌灵、噻菌灵和甲霜灵残留[J]. 农药学学报, 2015, 17(5): 579-584. DOI: 10.3969/j.issn.1008-7303.2015.05.11
    Li Chunli, Le Yuan, Yin Guihao, Yang Xinfeng, Li Shuhuai, Liu Chunhua. Determination of carbendazim,thiabendazole and metalaxyl residues in wax-apple by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2015, 17(5): 579-584. DOI: 10.3969/j.issn.1008-7303.2015.05.11
    Citation: Li Chunli, Le Yuan, Yin Guihao, Yang Xinfeng, Li Shuhuai, Liu Chunhua. Determination of carbendazim,thiabendazole and metalaxyl residues in wax-apple by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2015, 17(5): 579-584. DOI: 10.3969/j.issn.1008-7303.2015.05.11

    超高效液相色谱-串联质谱法测定莲雾中多菌灵、噻菌灵和甲霜灵残留

    Determination of carbendazim,thiabendazole and metalaxyl residues in wax-apple by ultra performance liquid chromatography-tandem mass spectrometry

    • 摘要: 建立了莲雾中多菌灵、噻菌灵和甲霜灵残留的超高效液相色谱-串联质谱(UPLC-MS/MS)的快速检测方法。样品直接用乙腈匀浆提取,过0.22 μm滤膜后,在电喷雾正离子模式下以多反应监测(MRM)模式测定,基质匹配标准溶液外标法定量。结果表明:方法的线性范围为0.01~0.5 μg/mL,决定系数(R2)>0.99;在0.04、0.4和2 mg/kg 3个添加水平下,方法的平均回收率为75%~107%,相对标准偏差为2.0%~8.9%(n=5),定量限均为0.04 mg/kg。该方法样品前处理简单、快速,分析时间短,灵敏度、准确度和精密度均符合农药残留检测要求。

       

      Abstract: A rapid method for determining carbendazim, thiabendazole and metalaxyl residue in wax-apples was developed with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) detection. The samples were extracted with acetonitrile. The samples were detected by UPLC-MS/MS under positive electrospray ionization and multiple reaction monitoring mode. The matrix-matched external standard calibration curves were used for the quantitative analysis. It was shown that the calibration curves were linear in the range of 0.01-0.5 μg/mL and coefficient of determination R2>0.99.The limits of quantitation were 0.04 mg/kg. The average recoveries of the three pesticides were 75%-107% at spiked levels of 0.04, 0.4 and 2 mg/kg, with relative standard deviations in the range of 2.0%-8.9% (n=5). The sample pretreatment of the method is simple and time-saving. The method is applied for detection of carbendazim, thiabendazole and metalaxyl residues in market wax-apples.

       

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