Determination of neonicotinoid insecticides in fruits and vegetables by ultra-high performance liquid chromatography-tandem mass spectrometry
Objective To establish an ultra-high performance liquid chromatography-mass spectrometry(UPLC-MS/MS)method for the determination of residues of 12 neonicotinoid insecticides(imidacloprid,acetamiprid,thiamethoprid,thiamethoxam,thiamethoxam,clothianidin,dinotefuran,nitenpyram,imidaclothiz,IPP,cycloxaprid,sulfoxaflor,flufuranone)in fruits and vegetables.Collect fruit and vegetable samples within Heilongjiang Province for testing,analyze data,and give constructive measures and suggestionsac-cording to the monitoring risk tips.Methods The samples were extracted with acetonitrile,purified by dispersive solid phase extraction using quick,easy,cheap,effective,rugged,safty(QuEChERS)pretreatment technique,determined by ultra-high performance liquid chromatography-mass spectrometry,detected by electrospray ionization(ESI+)multiple reaction monitoring(MRM)mode,quantified by external standard method and the results were analyzed,achieving simultaneous determination of residues of 12 neonicotinoid insecticides in fruits and vegetables.Results The linear ranges of 12 neonicotinoid insecticides were 5-200 ng/mL,with all the correlation coefficients＞0.999.The limits of detection was 0.001 mg/kg,and the limits of quantification was 0.005 mg/kg.Atspiked levels of 5,50 and 200 ng/mL,the average recoveries of the method ranged from 89.8％to 113.9％,with a relative standard deviation of 0.4％to 3.4％.Totally 107 samples were detected from 341 samples,with a detection rate of 31.4％.Conclusion The method is simple,rapid,accurate and sensitive.It can be used in batch measurement and has a good practical application prospect.
Neonicotinoid insecticidesFruits and vegetablesUltra high performance liquid chromatography-tandem mass spectrometry
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