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荔枝与龙眼中噻虫啉、螺虫乙酯及代谢物的高效液相色谱-串联质谱分析
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作者单位
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 
基金项目:国家重点研发计划项目(2016YFD0200206-Y);国家荔枝龙眼产业技术体系资助(CARS-32-16)
中文摘要: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1~500 μg/L,相关系数(r2)均大于0.990,检出限(LOD)为0.03~0.3 μg/kg,定量下限(LOQ)为0.1~1.5 μg/kg。荔枝和龙眼中噻虫啉、螺虫乙酯及4种代谢物在1、10、100 μg/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。
中文关键词:高效液相色谱-串联质谱  QuEChERS  噻虫啉  螺虫乙酯及代谢物  荔枝  龙眼
 
Determination of Thiacloprid,Spirotetramat and Its Metabolites Residues in Litchi and Longan by High Performance Liquid Chromatography-Tandem Mass Spectrometry
Abstract: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.
Key Words:high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)  QuEChERS  thiacloprid  spirotetramat and its metabolites  litchi  longan
引用本文:王思威,曾广丰,刘艳萍,王潇楠,孙海滨.荔枝与龙眼中噻虫啉、螺虫乙酯及代谢物的高效液相色谱-串联质谱分析[J].分析测试学报,2019,(2):201-206.
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