液-质联用法测定唑菌酯在土壤中的残留

Determination of Pyrazoxystrobin Residues in Soil by LC-MS/MS

[目的]建立唑菌酯在土壤中的残留分析方法。[方法]用乙腈对土壤样品进行超声提取,提取液经稀释后用液-质联用法进行分析测定。[结果]唑菌酯在0.05~5.0μg/L质量浓度范围内具有良好的线性关系,相关系数为0.9957,当添加质量分数为0.02~2.0 mg/kg,唑菌酯在3种土壤中的添加平均回收率为86.8%~102.9%,相对标准偏差为1.6%~5.6%。方法最小检出量为5.0×10^(-13)g,土壤中最低定量限(LOQ)为0.02 mg/kg。[结论]该方法灵敏度高,操作简单,准确度及精密度均满足农药残留分析的要求,适用于土壤中唑菌酯残留量的测定。

[Aims] A LC-MS/MS method for determination of pyrazoxystrobin residues in soil was established. [Methods] The pyrazoxystrobin residues in soil samples were extracted with acetonitrile by ultrasonic method, the extract was diluted and analyzed by LC-MS/MS. [Results] The calibration curve was linear in the range of 0.05 to 5.0 μg/L, and the correlation coefficient was 0.9957. When the fortified levels were ranged from 0.02 to 2.0 mg/kg, the average fortified recoveries in three kinds of soil were in the range of 86.8 to 102.9%, and the relative standard deviations were 1.6-5.6%. The limit of detection for pyrazoxystrobin was 5.0 × 10-13 g, and the limit of quantification was 0.02 mg/kg. [Conclusions] The method has the advantage of simple and high sensitivity. The accuracy and precision were satisfied the requirement of pesticide residues analysis, which could be applied for the determining pyrazoxystrobin residue in soil.