超高效液相色谱-串联质谱法测定豇豆中溴氰虫酰胺等5种农药残留

Using ultra performance liquid chromatography-tandem mass spectrometry to analyze 5 pesticide residues in cowpea

建立了超高效液相色谱-串联质谱（ UPLC-MS/MS）同时测定豇豆中溴氰虫酰胺、乙基多杀菌素、呋虫胺、噻虫嗪和啶虫脒残留量的方法。豇豆样品经乙腈提取，通过QuEChERS法净化后，采用Acquity UPLC？？ BEH C18色谱柱分离，在电喷雾正离子模式下以多反应监测（ MRM）模式检测。结果表明：在0.01~1μg/mL内5种农药的峰面积与其相应的质量浓度间呈良好线性关系，相关系数均大于0.99；在0.01、0.1和1 mg/kg 3个添加水平下，回收率为71％~129％，相对标准偏差为0.90％~20.8％（ n ＝5）。5种农药在豇豆中的检出限为0.084~4.0μg/kg，定量限为0.80~16.6μg/kg。该方法简单灵敏，定量准确，可用于分析豇豆中的溴氰虫酰胺、乙基多杀菌素、呋虫胺、噻虫嗪和啶虫脒的残留量。

A simple and efficient method based on QuEChERS sample cleanup and ultra performance liquid chromatography-tandem mass spectrometry（ UPLC-MS/MS） detection was developed to analyze residues of cyantraniliprole, spinetoram, dinotefuran, thiamethoxam and acetamiprid in cowpea simultaneously. The samples were homogenized and extracted with acetonitrile. After QuEChERS cleanup, the retention of target compounds was performed on an Acquity UPLC？？ BEH C18 column by gradient elution. The qualitative and quantitative analyses of 5 pesticides were operated with electrospray ionization mass spectrometry under positive mode using multiple reaction monitoring＆nbsp;（ MRM） mode. The results showed that the correlation coefficients of calibration curves were over 0. 99 in linear range. The average recoveries of the 5 pesticides at three spiked concentration levels （0. 01, 0. 1 and 1 mg/kg） varied from 71% to 129% with relative standard deviations （ RSDs） of 0. 90% -20. 8%（ n =5 ） . The limits of detection （ LOD ） and quantitation （ LOQ ） were 0. 084 -4. 0 μg/kg and 0. 80-16. 60μg/kg, respectively. In conclusion, this simple and efficient method met the method validation requirements for the determination of these 5 pesticide residues in cowpea.