QuEChERS-超高效液相色谱-串联质谱法测定土壤中10种酰胺类除草剂残留量

Determination of ten amide herbicide residues in soil by QuEChERs-ultra high performance liquid chromatography-tandem mass spectrometry

采用QuEChERS方法结合超高效液相色谱-串联质谱法测定土壤中10种酰胺类除草剂残留量。土壤样品经水和乙腈提取,4 g无水硫酸镁和1 g氯化钠盐析,100 mg PSA净化后用UPLC-MS/MS测定。质谱采用正离子电离和多反应监测模式(MRM),基质匹配标准溶液外标法定量。10种酰胺类除草剂在各自的浓度范围内线性关系良好(r^2>0.99)。10种酰胺类除草剂在高、中、低3个添加水平下,回收率为82.7%～114.2%,RSD为1.1%～8.5%,方法的定量限为0.5～100μg/kg。该方法操作简单、快速、灵敏度和准确度高,适合土壤样品中10种酰胺类除草剂多残留的检测分析。

A new method was adopted for the simultaneous determining of 10 amide herbicide residues in soil by UPLC-MS/MS. The soil samples were extracted by water and acetonitrile, and salted out with 4 g magnesium sulfate and 1 g sodium chloride, then cleaned up by 100 mg primary secondary amine (PSA), the purified extracts were detected by UPLC-MS/MS with positive mode and multiple reactions monitoring (MRM) mode and quantified by matrix-matched external standard calibration curves. The calibration curves of 10 amide herbicide residues showed good linearity. The correlation coefficients were higher than 0.99 and the recoveries of the 10 amide herbicide residues at three spiked levels ranging from 82.7% to 114.2% with the relative standard deviations (RSDs) from 1.1% to 8.5%.The limits of quantification were in the range of 0.5-100 μg/kg. The method is simple, time-saving, sensitive and accurate, and suitable for qualitative and quantitative analysis of the 10 amide herbicide residues in soil.