土壤中拟除虫菊酯类残留农药的气相色谱测定方法研究
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* 国家重点基础研究发展规划(973)项目(2002CB410805)资助


DETERMINATION OF RESIDUES OF PYRETHROID INSECTICIDES IN SOIL BY CAPILLARY GAS CHROMATOGRAPHY
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    摘要:

    建立了土壤中氯氰菊酯、氰戊菊酯和溴氰菊酯的提取、净化以及毛细管气相色谱的测定方法。运用石油醚-丙酮(V/V,2:1)混合溶剂提取,用氟罗里硅土进行层析净化,60ml石油醚/乙酸乙酯(V/V,9:1)进行洗脱,电子捕获-气相色谱测定,单点外标法定量。实验表明:土样中添加0.08mgkg-1的氯氰菊酯、氰戊菊酯和溴氰菊酯3种农药混标时,方法回收率为89.67%~90.62%,添加0.40mgkg-1时,方法回收率为91.07%~93.02%;操作中相对标准偏差(RSD)为2.02%~3.70%,最小检出量可达1.00pg。在检测色谱精密度实验中,5次测定3种农药混标,相对标准偏差(RSD)为1.37%~2.88%。实验表明,该法具有灵敏度高、操作简便、净化效果好、重现性好等特点。

    Abstract:

    A method for extracting,clearing off and determining residues of cypermethrin,fenvalerate and deltamethrin in soil has been developed.The method uses pertole mether-acecton (V/V,2:1) mixture to extract residues of the pesticides in soil samples,a column (20 cm×1.5 cm) packed with 3g Florisil to clear the mixture of the residues,and pertolem ether-ethyl acetate (V/V,9:1) to elute the residues from the column.Then the eluent is determined by gas chromatography (ECD-GC) with a HP-5 (30 m×0.32 mm×0.25 μ m) capillary column and quantified by the single pointexternal standard method.In an experiment of using this method,the recovery rates of cypermethrin,fenvalerate and deltamethrin were found to be 90.10%~93.02%,90.62%~91.07% and 89.67%~91.53% respectively with RSD being 2.02%~2.49%,2.51%~3.70% and 3.08%~3.42%,respectively in the operation.And the minimum detectable quantity was 1.00 pg.The relative standard deviations (n=5) of the equipment ranges from 1.37% to 2.88%.This method is proved to be easy in operation,and high in sensitivity,reproductivity and selectivity.

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陈莉,章钢娅,靳伟,胡锋.土壤中拟除虫菊酯类残留农药的气相色谱测定方法研究[J].土壤学报,2006,43(5):764-771. DOI:10.11766/trxb200505110509 Chen Li, Zhang Gangya, Jin Wei, Hu Feng. DETERMINATION OF RESIDUES OF PYRETHROID INSECTICIDES IN SOIL BY CAPILLARY GAS CHROMATOGRAPHY[J]. Acta Pedologica Sinica,2006,43(5):764-771.

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  • 收稿日期:2005-05-11
  • 最后修改日期:2005-09-28
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  • 在线发布日期: 2013-02-25
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