QuEChERS/超高效液相色谱-串联质谱法测定土壤中31种磺酰脲类除草剂残留

Determination of 31 Sulfonylurea Herbicide Residues in Soil by QuEChERS/Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了一种基于QuEChERS前处理技术和超高效液相色谱-串联质谱(UHPLC-MS/MS)同时测定土壤中31种磺酰脲类除草剂残留的方法。通过对色谱条件、提取溶剂、净化剂等进行优化,确定以甲醇和0.1%甲酸+5 mmol/L乙酸铵为流动相,1%(体积分数)乙酸-乙腈为提取溶剂,C18(25.00 mg/mL)为净化剂。31种磺酰脲类除草剂的线性关系良好,相关系数(r2)均不小于0.998 0,定量下限(S/N=10)为0.012~2.321μg/kg。3个加标水平(10、100、400μg/kg)下的平均回收率为71.8%~119%,相对标准偏差(RSD)为0.62%~13%。除烟嘧磺隆、三氟啶磺隆钠、玉嘧磺隆、啶嘧磺隆、氯吡嘧磺隆为中等强度基质效应外,其余待测物均表现为弱基质效应。该方法简便易操作,具有较好的灵敏度和准确度,适用于土壤中31种磺酰脲类除草剂残留的同时检测。

A method based on QuEChERS pretreatment technique and ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS) was developed for the simultaneous determination of 31 sulfonylurea herbicide residues in soil.After optimizing the pretreatment and chromatographic conditions,methanol and 0.1% formic acid +5 mmol/L ammonium acetate,1% acetic acid-acetonitrile and 25.00 mg/mL C18 were used as the mobile phases,extraction solvents and purification agents,respectively.There were good linear relations for 31 sulfonylurea herbicides with their correlation coefficients(r2) no less than 0.998 0.The limits of quantitations(S/N=10) were in the range of 0.012-2.321 μg/kg.Average recoveries for the analytes at three spiked levels of 10,100 and 400 μg/kg ranged from 71.8% to 119% with their relative standard deviations(RSD) of 0.62%-13%.Except for nicosulfuron,trifloxysulfuron sodium,rimsulfuron,flazasulfuron and halosulfuron methyl,other compounds showed weak matrix effects.With easy operation,good sensitivity and accuracy,this method is suitable for the simultaneous detection of 31 sulfonylurea herbicide residues in soil.