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分散固相萃取—气相色谱法测定稻谷中5种有机磷农药残留
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Determination of 5 organophosphorus pesticides residues in paddy by dispersive solid phase extraction- gas chromatography
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    摘要:

    建立中性氧化铝分散固相萃取—火焰光度气相色谱法测定稻谷中乐果、毒死蜱、马拉硫磷、水胺硫磷、三唑磷5种有机磷农药残留量的分析方法。样品粉碎后经乙腈提取,中性氧化铝分散萃取,萃取液于70 ℃水浴中氮吹干,丙酮定容后用带火焰光度检测器的毛细管气相色谱仪(GC-FPD)测定。结果表明,5种有机磷在0.05~5.00 μg/mL范围具有良好的线性关系,乐果、毒死蜱、马拉硫磷、水胺硫磷、三唑磷的线性相关系数均为0.999 9,检出限(LOD)为0.002 mg/kg,最低定量限(LOQ)为0.007 mg/kg。稻谷样品中低、中、高3个质量浓度的添加回收率在97.7%~108.0%之间,相对标准偏差(RSD,n=6)在0.8%~5.7%之间。方法可以满足稻谷中5种有机磷农药残留一次处理同时分析检测的要求。

    Abstract:

    A fast method was developed for the determination of 5 organophosphorus pesticide residues (dimethoate, chlorpyrifos, malathion, isocarbophos, fenitrothion) in paddy by neutral alumina dispersive solid phase extraction - gas chromatography with flame photometric detector (DSPE-GC-FPD). The powdered samples were extracted with acetonitrile. The extract was purified by neutral alumina DSPE,dried by nitrogen evaporator with water bath at 70 ℃,and dissolved by acetone and determined by capillary gas chromatograph with flame photometric detector(CGC-FPD). The results showed that the 5 organophosphorus pesticide showed a good linear relationship in the range of 0.05~5.00 μg/mL, all of their linear correlation coefficients were 0.999 9, the limit of detection was 0.002 mg/kg, and the minimum quantitative limit was 0.007 mg/kg. The spiked recoveries at three levels of standard additions in paddy were between 97.7%~108.0%, and the RSDs (n=6) were between 0.8%~5.7%. This method could be used to determine 5 organophosphorus pesticide residues in paddy at the same time.

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徐明雅,潘丹杰,杨志成,张烝彦.分散固相萃取—气相色谱法测定稻谷中5种有机磷农药残留[J].粮油食品科技,2015,23(4):75-79.

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  • 在线发布日期: 2015-09-02
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