氯氟吡氧乙酸异辛酯和氯氟吡氧乙酸在玉米植株及土壤上的残留分析方法

Analysis of Fluroxypyr-meptyl and Fluroxypyr Residues in Corn Plant and Soil

[目的]建立气相色谱法和超高效液相色谱串联质谱法分别检测玉米植株和土壤中氯氟吡氧乙酸异辛酯和氯氟吡氧乙酸残留的分析方法。[方法]植株和土壤中的氯氟吡氧乙酸异辛酯和氯氟吡氧乙酸均经乙腈提取,氯氟吡氧乙酸异辛酯通过柱层析法净化,气相色谱仪检测;氯氟吡氧乙酸经QuEChERS法净化,利用超高效液相色谱-串联质谱(UPLC-MS/MS)测定,采用电喷雾负离子模式(ESI-),在多反应监测(MRM)模式下进行检测,基质匹配外标法定量。[结果]氯氟吡氧乙酸异辛酯在0.05~2.0 mg/L质量浓度范围内线性关系良好,相关系数为0.9997,在0.025~0.5 mg/L添加水平范围内,植株和土壤中的平均回收率为89.9%~100.6%,相对标准偏差为5.2%~10.2%,最低检出量为4.7×10^(-4)ng;氯氟吡氧乙酸在0.01~1.0 mg/L质量浓度范围内线性关系良好,相关系数为0.9995,在0.025~0.5 mg/kg添加水平范围内,植株和土壤的平均回收率为73.6%~92.8%,相对标准偏差为1.3%~9.4%,最低检出量为2.3×10^(-2)ng。[结论]建立方法的灵敏度、准确度和精确度均符合农药残留分析的要求,适用于玉米植株和土壤中氯氟吡氧乙酸异辛酯和氯氟吡氧乙酸的检测和确证。

[Aims] A new method for analysis of fluroxypyr-meptyl and fluroxypyr residues in com plant and soil by gas chromatography and ultra performance liquid chromatography-tandem mass spectrmn respectively was developed. [Methods] The fluroxypyr-meptyl and fluroxypyr in corn plant and soil were extracted with acetonitrile. Fluroxypyr-meptyl was cleaned up by column chromatography and determined by GC. Fluroxypyr was purified by QuEChERS method, detected by UPLC-MS/MS under negative electrospray ionation （ESI） and multiple reaction monitoring （MRM） mode with matrix matching and quantification of external standard method. [Results] The results showed that when the concentration ranged from 0.05 to 2.0 mg/L, the method for fluroxypyr-meptyl displayed good linearity with the correlation coefficient of 0.9997. When the fortified levels ranged from 0.025 to 0.5 rag/L, the average fortified recoveries were in the range of 89.9 to 100.6% and the relative standard deviations were in the range of 5.2 to 10.2%, the limits of detection for fluroxypyr-meptyl was 4.7×10^-4 ng. When the concentration ranged from 0.01 to 1.0 mg/L, the method for fluroxypyr displayed good linearity with the correlation coefficient of 0.9995. When the fortified levels ranged from 0.025 to 0.5 mg/L, the average fortified recoveries were in the range of 73.6 to 92.8% and the relative standard deviations were in the range of 1.3 to 9.4%, the limits of detection for fluroxypyr was 2.3 ×10^-2 ng. [Gonelusions] The method is simple and reliable, meets with the requirement for pesticide residue analysis, which is suitable for determination of fluroxypyr-meptyl and fluroxypyr in corn plant and soil.