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

作　　者：钱程[1,2,3] 吴琼[1,2] 吕岱竹[1,2] 李建国[1,2] 

机构地区：[1]中国热带农业科学院 析测试中心,海口571101 [2]海南省热带果蔬产品质量安全重点实验室,海口571101 [3]华中农业大学,武汉430070

出　　处：《农药学学报》2014年第5期594-599,共6页Chinese Journal of Pesticide Science

基　　金：公益性行业(农业)科研专项(201303088-13)

摘　　要：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.

关 键 词：超高效液相色谱-串联质谱 豇豆 溴氰虫酰胺 乙基多杀菌素 呋虫胺 噻虫嗪 啶虫脒 残留 ultra liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) 

分 类 号：S482.3[农业科学—农药学] TQ450.2[农业科学—植物保护]