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建立了超高效液相色谱—串联质谱仪测定稻田环境中的丙草胺和西草净的残留分析检测方法。糙米、稻壳、植株、土壤以及田水样品中的丙草胺和西草净以乙腈为提取剂,N-丙基乙二胺(PSA)净化,采用超高效液相色谱—串联质谱测定。丙草胺在0.01~5.0 mg/L范围内线性良好,相关系数为0.997 4,丙草胺在糙米、稻壳、植株、土壤以及田水中的平均加标回收率为71.8%~103.6%,相对标准偏差为1.7%~9.2%;西草净在0.005~2.5 mg/L范围内线性良好,相关系数为0.997 9,西草净在不同样品中的平均加标回收率为75.0%~107.3%,相对标准偏差在1.7%~11.9%之间。该方法重复性好,准确度、精密度均能满足农药残留量分析与检测的技术要求。
A method for the determination of residues of pretilachlor and simethicone in paddy field by ultra performance liquid chromatography-tandem mass spectrometry was established. In the brown rice, rice husk, plant, soil and field water samples, pretilachlor and simethicone were extracted with acetonitrile and purified with N-propyl ethylenediamine (PSA) using ultra performance liquid chromatography-tandem mass spectrometry. In the range of 0.01-5.0 mg / L, pretilachlor had a good linearity with a correlation coefficient of 0.997 4. The average recoveries of pretilachlor in brown rice, rice husk, plant, soil and field water ranged from 71.8% to 103.6% The standard deviation ranged from 1.7% to 9.2%. The calibration curve was linear over the range of 0.005-2.5 mg / L, with a correlation coefficient of 0.997 9. The average spiked recoveries of simethicone in different samples ranged from 75.0% to 107.3% The relative standard deviation was between 1.7% and 11.9%. The method has good repeatability, accuracy and precision to meet the technical requirements of pesticide residue analysis and detection.