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| Determination of 127 Pesticide Residues in Cucumber,Flowering Cabbage,Grape and Banana by QuEChERS Method Coupled with High Performance Liquid Chromatography Tandem Mass Spectrometry |
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| DOI：10.3969/j.issn.1004-4957.年份.月份 |
| KeyWord:QuEChERS high performance liquid chromatography tandem mass spectrometry（HPLC-MS/MS） fruits and vegetables pesticide residues |
| Author | Institution |
| LI Rong,CHU Da-ke,ZHANG Peng-jie,GAO Yong-qing,HUANG Si-yun |
1.中山出入境检验检疫局;2.广东药学院食品科学学院 |
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| Abstract: |
| A rapid method was developed for the simultaneous determination of 127 pesticide residues belonging to different chemical classes in cucumber,flowering cabbage,grape and banana by high performance liquid chromatography tandem mass spectrometry（HPLC-MS/MS）.The samples was prepared by the modified QuEChERS（quick,easy,cheap,effective,rugged and safe） method,extracted with acetonitrile containing 1% acetic acid,salted out with anhydrous magnesium sulphate and anhydrous sodium acetate,and cleaned up by adding primary secondary amine（PSA） and graphitized carbon black（GCB）.The 127 target compounds were separated on an Ultra AQ C18（100 mm×2.1 mm,3 μm） column using 5 mmol/L ammonium formate methanol solution and 5 mmol/L ammonium formate as mobile phase by gradient elution at a flow rate of 0.4 mL/min in 15 min,and analyzed by positive electrospray ionization tandem mass spectrometry under multiple reaction monitoring（MRM） mode.The external standard method was used for quantitative analysis.The calibration curves of 127 pesticide residues were linear in the range of 0.50-40.0 μg/L with correlation coefficients（r） more than 0.99．The recoveries at spiked levels of 10,20,50 μg/kg for all target compounds in the samples were in the range of 60.0%-118.5%,with relative standard deviations of 1.2%-21.9%.The limits of quantitation（LOQs，S/N≥10） were not more than 8.9 μg/kg.The method was simple,rapid,sensitive and reliable,and could be used in the screening and determination of 127 pesticide residues in fruits and vegetables. |
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