摘要
建立了QuEChERS-UPLC-MS/MS法快速同时检测番茄中噻虫嗪及其代谢产物(噻虫胺)、螺虫乙酯及其4种代谢产物(BYI08330-enol-glucoside、BYI08330-mono-hydroxy、BYI08330-enol和BYI08330-ketohydroxy)残留的分析方法。样品经乙腈提取,NaCl和无水Mg SO4除水后,经N-丙基乙二胺(PSA)和C18粉末净化,用超高效液相色谱-串联质谱(UPLC-MS/MS)分析,采用多反应离子监测模式(MRM)检测,基质匹配标准溶液外标法定量。7种目标物质在0.2~2 000μg/L质量浓度范围内均具有良好的线性关系(r2≥0.999 2),在0.002、0.02、0.20、2.00 mg/kg加标水平下的平均回收率为79.9%~104%,相对标准偏差(RSD)为0.94%~6.4%,方法定量下限(LOQ)为0.002 mg/kg。该方法快速简便、灵敏度高、重现性好,能满足番茄中噻虫嗪、噻虫胺和螺虫乙酯及其代谢产物残留的快速检测和确证要求。
In this study,an analytical method was established for the determination of thiamethoxam and its metabolites clothianidin,spirotetramat and its four metabolites such as BYI08330-enol-glucoside,BYI08330-ketohydroxy,BYI08330-enol and BYI08330-mono-hydroxy residues in tomatoes using QuEChERS cleanup with ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）.The residues in samples were extracted with acetonitrile,dehydrated with anhydrous magnesium sulfate and sodium chloride,then purified with primary secondary amine （PSA） sorbent and C18,finally detected by ultra-performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） under the multi-reactive ion monitoring mode（MRM） and quantified by external standard method.The results showed that good linearities for the seven analytes i.e.thiamethoxam,clothianidin,spirotetramat,BYI08330-enol-glucoside,BYI08330-mono-hydroxy,BYI08330-enol and BYI08330-ketohydroxy were observed in the concentration range of 0.2-2 000 μg/L with the correlation coefficients（r2） not less than 0.999 2. The limits of quantification（LOQs） were 0.002 mg/kg.The average recoveries at the fortified levels of 0.002,0.02,0.20 and 2.00 mg/kg were in the range of 79.9%-104% with the relative standard deviations of 0.94%-6.4%.With the advantages of rapidness,simplicity,high sensitivity and good reproducibility,the method is suitable for the determination of thiamethoxam,clothianidin,spirotetramat and their four metabolites residues in tomatoes.
出处
《分析测试学报》
CAS
CSCD
北大核心
2017年第12期1431-1438,共8页
Journal of Instrumental Analysis
基金
2017年国家柑桔及热带作物产品质量安全风险评估项目(GJFP2017004)
国家现代农业(柑桔)产业技术体系建设项目(CARS-26)
