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磁基QuEChERS结合HPLC-MS/MS法测定10种烟草农药残留

Determination of 10 tobacco pesticide residues by magnetic QuEChERS combined with HPLC-MS/MS

  • 摘要: 为建立一种磁基QuEChERS结合液相色谱-串联质谱测定10种烟草农药残留的分析方法,以磁性碳材料(Fe3O4@C)为净化吸附剂,考察了不同温度煅烧制备的Fe3O4@C对方法回收率的影响,并系统评估了其应用效果。结果表明:①10种农药测定的线性质量浓度范围为2~200 μg/L,线性关系良好,相关系数均大于0.992。②在3个加标水平(20、50和200 μg/kg)下的平均回收率均在80.6%~105.9%范围内,相对标准偏差(n=6)均小于13.4%,10种农药的检测限为0.05~0.67 μg/kg,定量限为0.18~2.23 μg/kg。该方法准确度高、灵敏度好,且可通过Fe3O4@C的磁回收性能简化前处理过程,适用于10种烟草农药残留的定量分析。

     

    Abstract: To develop an analytical method combining magnetic QuEChERS and liquid chromatography- tandem mass spectrometry for the determination of 10 tobacco pesticide residues using magnetic carbon material (Fe3O4@C) as a purification adsorbent, the effects of Fe3O4@C prepared at different calcination temperatures on pesticide recovery were investigated and the application performance of Fe3O4@C was further systematically evaluated. The results showed that: 1) Good linearity (R > 0.992) was obtained for all the target pesticides at concentrations of 2-200 μg/L. 2) The repeatability for all the target pesticides at three spiked concentrations of 20, 50 and 200 μg/kg was satisfactory (RSD < 13.4%, n=6) and the recoveries ranged from 80.6% to 105.9%. The limits of detection (LODs) and limits of quantitation (LOQs) ranged from 0.05 to 0.67 μg/kg and from 0.18 to 2.23 μg/kg, respectively. The developed method is accurate and sensitive, simplifies the pretreatment process by magnetic recovery of Fe3O4@C, and is suitable for the quantitative analysis of 10 tobacco pesticide residues.

     

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