张雪燕, 代雪芳. 四聚乙醛在烟草和土壤中的残留检测与消解动态[J]. 农药学学报, 2006, 8(4): 344-348.
    引用本文: 张雪燕, 代雪芳. 四聚乙醛在烟草和土壤中的残留检测与消解动态[J]. 农药学学报, 2006, 8(4): 344-348.
    ZHANG Xue-yan, DAI Xue-fang. Degradation and Determination of the Residue of Metaldehyde in Tobacco and Soil[J]. Chinese Journal of Pesticide Science, 2006, 8(4): 344-348.
    Citation: ZHANG Xue-yan, DAI Xue-fang. Degradation and Determination of the Residue of Metaldehyde in Tobacco and Soil[J]. Chinese Journal of Pesticide Science, 2006, 8(4): 344-348.

    四聚乙醛在烟草和土壤中的残留检测与消解动态

    Degradation and Determination of the Residue of Metaldehyde in Tobacco and Soil

    • 摘要: 建立了烟草和土壤中四聚乙醛残留量的气相色谱分析方法。样品中残留的四聚乙醛用二氯甲烷提取,中性氧化铝与活性炭混合柱净化,偏重亚硫酸钠溶液除去游离醛,所得的四聚乙醛经盐酸解聚成乙醛,乙醛与2,4-二硝基苯肼进行衍生化反应,经硅胶柱净化,GC-NPD测定其衍生物。方法的最小检出量为0.04 ng,最低检出浓度为0.02~0.10 mg/kg;3个添加水平的平均回收率为86%~100%,相对标准偏差(RSD)均小于15%(n=5)。四聚乙醛在烟草及土壤中的残留试验结果表明:烟草植株对四聚乙醛的吸收在施药后4~5 d达到高峰,之后缓慢下降,到21 d已接近最低检出浓度0.04 mg/kg;其在土壤中的半衰期约为4 d;在推荐使用剂量下,四聚乙醛在干烟叶中的残留量低于最低检出浓度0.10 mg/kg,不会对烟草造成残留污染。

       

      Abstract: A method for determination of metaldehyde residues in tobacco was developed. Metaldehyde residues were extracted from tobacco with dichloromethane and cleaned up with the mixture column of aluminum oxide-activated carbon.Interfering aldehydes were removed with sodium meta-bisulphite solution.Metaldehyde was depolymerized with hydrochloric acid to acetaldehyde, which was reacted with 2,4-dinitrophenylhydrazine.The derivative acetaldehyde 2,4-dinitrophenylhydrazone was cleaned up on silica gel column and determined by GC-NPD.The limit of detection of metaldehyde was 0.04 ng.The limit of quantification of the method for pesticide in tobacco and soil was 0.02 to 0.10 mg/kg.The recoveries from 3 samples fortified with metaldehyde at levels of 0.02 to 1.0 mg/kg, ranged from 86% to 100%.And the RSD was below 15%(n=5).The study of the residue dynamics demonstrated that: 1) The absorption of metaldehyde was the highest 4 days after treatment, and then the absorption declined slowly.After 21 days, the residues of metaldehyde was 0.04 mg/kg nearing the limit of quantification.The half life of metaldehyde was 4 days in soil.2) When metaldehyde was used as the recommended dosage,the residues of metaldehyde was below 0.10 mg/kg in dry tobacco,thus no any contamination to tobacco product.

       

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