菊薯中3种硫代磷酸酯类有机磷农药残留量的快速测定
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国家“十二五”科学支撑计划项目(2011BAI06B03)


Rapid determination of three phosphorothioate pesticides in yacon
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    摘要:

    应用超分子印迹微球与逆基质固相分散加速溶剂萃取,采用气相色谱质谱(GC-MS)检测方法测定菊薯中3种硫代磷酸酯类有机磷农药(毒死蜱、喹硫磷和甲基立枯磷)残留量。以甲基立枯磷为模板分子制备对3种农药有特异性识别的分子印迹微球聚合物, 然后作为固相分散剂进行加速溶剂萃取, 再以气相色谱质谱法测定菊薯中3种农药的残留量, 质谱条件为电子轰击离子源正离子选择离子监测模式。结果表明:3种农药的线性范围均为0.01~2.50 μg/mL,相关系数为0.9987~0.9996; 3种农药的检出限范围为0.174~0.526 μg/kg,相对标准偏差为2.3%~9.9%,回收率为79.8%~104.5%。

    Abstract:

    This study developed a method to assess the levels of three phosphorothioate pesticides (chlorpyrifos, tolclofos-methyl,quinalphos) in yacon that based on using a molecularly imprinted reversed matrix solid-phase dispersion (MI-MSPD) and accelerated solvent extraction (ASE) combined with GC-MS. The MIPs are cross-linked polymers with specific binding sites for a particular analyte, which recognize target molecules by imprinting a molecule during polymer synthesis through covalent or non-covalent interactions. The obtained MIPs was used to extract and preconcentrate three phosphorothioate pesticides as adsorbent of matrix solid phase dispersion from yacon sample in extraction pot and cell of ASE, then the samples were detected by gas chromatography-mass spectrograph(GC-MS),and the positive ion mode of selected ion monitoring (SIM) with electron impact ionization source was adopted in MS. The results of 3 kinds of phosphorothioate agrochemicals identified in yacon samples in Wuhan area were satisfactory. The linear correlation was 0.9987-0.9996 between concentrations range of 0.01-2.5 μg/mL; the detection limit of the method was 0.174-0.526 μg/kg in yacon samples,the relative standard deviations were in the range of 2.3%-9.9% in yacon samples,the recoveries were in the range of 79.8%-104.5% in yacon samples.

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周梦春,何海,舒耀皋,王帆林,舒少华,王沫.菊薯中3种硫代磷酸酯类有机磷农药残留量的快速测定[J].华中农业大学学报,2015,34(4):31-36

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  • 收稿日期:2014-09-24
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  • 在线发布日期: 2015-06-02
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