[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。 [Objective] The research aimed to establish a method for the determination of iso-octyl fluride acetate and fluroxypyr in corn plants and soil by using gas chromatography and ultra performance liquid chromatography-tandem mass spectrometry. [Method] Isohexyl fluride and fluridyl acetate in plant and soil were extracted with acetonitrile and isooctyl fluride was purified by column chromatography and detected by gas chromatography; Oxyacetic acid was purified by QuEChERS method and detected by multi-reaction monitoring (MRM) mode using electrospray negative ion mode (ESI-) using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) Standard method of quantitative. [Result] The iso-octyl fumarate showed good linearity in the concentration range of 0.05-2.0 mg / L with the correlation coefficient of 0.9997. The average recovery of iso-octyl fumarate in the plant and soil ranged from 0.025 mg / L to 0.5 mg / L The relative standard deviations were 5.2% ~ 10.2% and the lowest detection limit was 4.7 × 10 ~ (-4) ng. The linear range of fluropepiride in the concentration range of 0.01 ~ 1.0 mg / L was 89.9% ~ 100.6% The correlation coefficient was 0.9995. Within the range of 0.025-0.5 mg / kg, the average recoveries of plant and soil ranged from 73.6% to 92.8% with relative standard deviations of 1.3% -9.4% and the lowest detection rates were 2.3 × 10 ~ (-2) ng. [Conclusion] The sensitivity, accuracy and precision of the established methods were all in accordance with the requirements of pesticide residue analysis. It was suitable for the detection and confirmation of isooctyl fenfluosyl acetate and fluropepiride in corn plants and soils.