QuEChERS/超高效液相色谱-串联质谱法同时测定土壤中67种农药残留

摘要

建立了同时测定土壤中67种农药的QuEChERS/超高效液相色谱-串联质谱法(QuEChERS/UPLC-MS/MS)方法.样品经乙腈振荡提取、QuEChERS净化,采用超高效液相色谱-串联质谱测定.质谱分析采用电喷雾电离,正负双离子扫描,多反应监测(MRM)模式.结果表明:67种农药在5～500 μg/L范围内均呈良好的线性关系,相关系数为0.990 ～0.999,检出限为0.001 ～0.010 mg/L;在10、50、500 μg/kg3个加标水平下的平均回收率为58％～111％,相对标准偏差(n=5)为1.1％～19.3％;定量下限为10 μg/kg.该方法简单、快速、重现性好、灵敏度高,可满足土壤中67种农药残留的检测要求.%A QuEChERS phase exaction coupled with ultra high performance liquid chromatographytandem mass spectrometric (QuEChERS/UPLC-MS/MS) method was developed for the simultaneous determination of 67 pesticide residues in soil.After extraction with acetonitrile,purification with QuEChERS cartridges and dissolution with methanol,the analytes in the sample solutions were analyzed by UPLC-MS/MS on an Agilent Proshell 120 EC-C18 column with a mixture of 0.1％ formic acid solution and acetonitrile as mobile phase by gradient elution.The mass spectrometer was operated in multiple reactions monitoring(MRM) mode under negative and positive modes.Good linearities were obtained for 67 pesticides in the concentration range of 5-500 μg/L with correlation coefficients more than 0.990 and detection limits of 0.001-0.010 mg/L.Recoveries for 67 pesticides at three spiked levels of 10,50,500 μg/kg were in the range of 58％-1 11％.The relative standard deviations(RSDs,n =5) were less than 20％,and the limits of quantitation were 10 μg/kg.The established method was simple,efficient and sensitive,and could be applied in the determination of 67 pesticide residues in soil.