UPLC-MS/MS法同时测定土壤中3种磺酰脲类除草剂残留

UPLC-MS/MS for simultaneous determination of three sulfonylurea herbicide residues in soil

建立了QuEChERS法一超高效液相色谱一串联质谱法（UPLC—MS／MS）快速测定土壤中噻吩磺隆、苯磺隆、氯嘧磺隆3种磺酰脲类除草剂的方法。采用振荡提取、QuEChERS法净化方法处理土壤样品，利用UPLC-MS／MS分析，在多反应监测（MRM）模式下以0．1％甲酸水和乙腈为流动相梯度洗脱。3种除草剂在0．5～500μg／L的质量浓度范围内线性关系良好，相关系数为：0．996—0．999。在10，50μg／kg水平下进行加标回收实验，平均回收率为81．4％-92．9％，RSD为5．5％～10．6％，方法检出限（S／N=3）为O．12～0．16μg／k。方法可用于大量实际土壤样品中3种除草剂的检测。

A method detecting 3 herbicide residues including thifensulfuron-methyl, tribenuron methyl, chlorimuron-ethyl in soil was established by using QuEChERS-ultra-high performance liquid chromatography- tandem mass spectrometry （UPLC-MS/MS）. Soil samples were rapidly extracted by acetonitrile, purified by C18 solid dispersant. The purified liquid was analysed by UPLC-MS/MS in multiple reaction monitoring （MRM） mode, and 0. 1% formic acid in water and acetonitrile were used as mobile phase to complete gradient elution. The calibration curves of three herbicides have good linear correlation in the concentration range of 0. 5 - 500 ng/mL （ R = 0. 996 -0. 999）. The spike recovery experiments were carried out at levels of 10μg/kg and 50 p.g/kg, the average recoveries were between 81.4% and 92. 9%, RSD were 5.5% - 10. 6%, and the method detection limit （SIN = 3） were 0. 12 ~ 0. 16 pg/kg. The results showed that the method could be used for the detection of the actual soil samples.