Determination of Thiacloprid,Spirotetramat and Its Metabolites Residues in Litchi and Longan by High Performance Liquid Chromatography-Tandem Mass Spectrometry
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KeyWord:high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)  QuEChERS  thiacloprid  spirotetramat and its metabolites  litchi  longan
WANG Si-wei,ZENG Guang-feng,LIU Yan-ping,WANG Xiao-nan,SUN Hai-bin 1.Guangdong Provincial Key Laboratory of High Technology for Plant Protection,Institute of Plant Protection,Guangdong Academy of Agricultural Sciences;2.Guangdong Inspection and Quarantine Technology Center
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      An analytical method was established for the determination of thiacloprid,spirotetramat and its four metabolites residues in litchi and longan by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) with QuEChERS cleanup.The residues in samples were extracted with acetonitrile,dehydrated with anhydrous magnesium sulfate and sodium chloride,then purified with C18 and GCB.The extract was separated on a Poroshell-120 EC-C18 column with 0.1% formic acid-acetonitrile as mobile phase by isocratic elution,detected by HPLC-MS/MS with positive electrospray ion source in multi reaction monitoring(MRM) mode,and quantified by external standard method.Results showed that there existed good linearities for six analytes in the range of 1-500 μg/L with their correlation coefficients(r2) more than 0.990.The limits of detection(LODs) and limits of quantitation(LOQs) were 0.03-0.3 μg/kg and 0.1-1.5 μg/kg,respectively.The average recoveries for the analytes at spiked levels of 1,10,100 μg/kg were in the range of 80.4%-99.5% with relative standard deviations of 1.4%-6.4%.The developed method was simple,sensitive,accurate and reliable,and could meet the requirements for rapid screening and monitoring of thiacloprid,spirotetramat and its metabolites in fruits such as litchi and longan.