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    低温提取气相色谱法测定大葱中辛硫磷

    Extraction of Phoxim in Welsh Onion Under Low Temperature and Its Determination by Gas Chromatography

    • 摘要: 建立了气相色谱法测定大葱中辛硫磷残留量的分析方法.大葱样品经冷冻后,采用约2 ℃乙腈提取,提取液盐析后浓缩供气相色谱分析.由于辛硫磷的热不稳定性,通过优化气相色谱条件,可减少热分解,提高响应值,辛硫磷的质量浓度在0.10~10.0 mg·L-1范围与峰面积呈线性关系(r=0.999 9),方法的检出限为0.01 mg·kg-1,在0.02~0.10 mg·kg-1添加水平回收率为83.1%~105.0%,相对标准偏差为2.6%~9.2%.

       

      Abstract: Residual phoxim in welsh onion was extracted with acetonitrile at about 2 ℃,and the extract was evaporated to nearly dryness after salting out with sodium chloride.The residue was taken up with 1 mL of acetone and was ready for GC determination.Considering the thermoinstability of phoxim,the conditions of gas-chromatography were optimized to reduce its thermo-decomposition and to raise response value.Linear relationship between the peak area and concentration of phoxim was kept in the range of 0.10-10.0 mg·L-1 (r=0.999 9),with its detection limit of 0.01 mg·kg-1.Recovery tests were made by addition of standard phoxim in the concentration range of 0.02 to 0.10 mg·kg-1,and the values of recovery obtained were in the range 88.1%-105.0%,and precision tests were also performed,giving values of RSD′s (n=6) in the range of 2.6%-9.2%.

       

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