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
王思威,曾广丰,刘艳萍,王潇楠,孙海滨 1.广东省农业科学院植物保护研究所广东省植物保护新技术重点实验室;2.广东检验检疫技术中心
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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.