作　　者： ; ; ;

机构地区： 广东省农业科学院

出　　处： 《分析测试学报》 2019年第2期201-206,共6页

摘　　要： 采用高效液相色谱-串联三重四极杆质谱结合QuEChERS前处理技术,建立了同时测定荔枝和龙眼中噻虫啉、螺虫乙酯及4种代谢物残留的分析方法。样品采用乙腈作为提取溶剂,经十八烷基键合硅胶(C18)与石墨化碳黑(GCB)吸附剂净化后,由Poroshell-120 EC-C18色谱柱分离,以0. 1%(体积分数)甲酸水溶液-乙腈为流动相等度洗脱,在电喷雾电离(ESI+)和多反应监测模式下进行检测,外标法定量分析。该方法的线性范围为1～500μg/L,相关系数(r^2)均大于0. 990,检出限(LOD)为0. 03～0. 3μg/kg,定量下限(LOQ)为0. 1～1. 5μg/kg。荔枝和龙眼中噻虫啉、螺虫乙酯及4种代谢物在1、10、100μg/kg加标水平下的平均回收率为80. 4%～99. 5%,相对标准偏差(RSD)为1. 4%～6. 4%。该方法操作简单、灵敏度高、准确性好、可靠性强,可满足荔枝和龙眼等水果中噻虫啉、螺虫乙酯及代谢物的快速筛查监测要求。 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 Qu EChERS 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 with0. 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( r^2) 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.

关 键 词： 高效液相色谱 串联质谱 噻虫啉 螺虫乙酯及代谢物 荔枝 龙眼

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