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Position: Home > Articles > Determination of Spirotetramat and Its 4 Metabolites in Citrus and Soil by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry Agrochemicals 2016 (1) 45-47

超高效液相色谱-质谱法测定柑橘和土壤中螺虫乙酯及4种代谢产物

作  者:
李菊颖;吴文铸;孔德洋;何健;陈全博;单正军
单  位:
环境保护部南京环境科学研究所国家环境保护农药环境评价与污染控制重点实验室
关键词:
螺虫乙酯;代谢产物;超高效液相色谱-串联质谱;Qu ECh ERS;柑橘
摘  要:
[目的]建立柑橘和土壤中螺虫乙酯及代谢产物BYI08330-enol-glucoside、BYI08330-ketohydroxy、BYI08330-enol和BYI08330-mono-hydroxy的残留分析方法。[方法]前处理方法利用乙腈为提取剂,N-丙基乙二胺(PSA)和石墨化炭黑(GCB)为分散净化剂的Qu ECh ERS方法,并利用超高效液相色谱-串联质谱(UPLC-MS/MS)在多反应离子监测模式(MRM)下进行检测,外标法定量。[结果]螺虫乙酯及4种代谢产物在0.002~0.500 mg/L质量浓度范围内均具有良好的线性关系(r2≥0.994);在0.01~1.00 mg/kg添加水平范围内平均回收率为70.7%~96.0%;相对标准偏差为1.2%~6.4%;方法检出限(LOD)在0.12~1.4μg/kg范围内;定量限(LOQ)在0.4~4.9μg/kg范围内。[结论]该方法分析速度快、灵敏度高、重现性好,适用于柑橘和土壤中螺虫乙酯及其代谢产物残留的快速检测和确证。
译  名:
Determination of Spirotetramat and Its 4 Metabolites in Citrus and Soil by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry
作  者:
LI Ju-ying;WU Wen-zhu;KONG De-yang;HE Jian;CHEN Quan-bo;SHAN Zheng-jun;Nanjing Institute of Environmental Sciences, Key Laboratory of Pesticide Environmental Assessment and Pollution Control,Ministry of Environmental Protection of the People's Republic of China;
关键词:
spirotetramat;;metabolite;;ultra performance liquid chromatography-tandem mass spectrometry;;QuEChERS;;citrus
摘  要:
[Aims] A method for the simultaneous determination of spirotetramat and its 4 metabolites such as BYI08330-enol-glucoside, BYI08330-ketohydroxy, BYI08330-enol and BYI08330-mono-hydroxy in citrus and soil was developed. [Methods] The residues in samples were extracted with acetonitrile and cleaned up by dispersive method with PSA and GCB as cleaning agents, then detected by ultra performance liquid chromatography-tandem mass spectrometry under multiple reaction monitoring mode, and quantified by external standard method. [Results] The results showed that the method has good linearity(r~2≥0.994) when the concentrations of spirotetramat and its 4metabolites were ranged from 0.002 to 0.500 mg/L. When the fortified levels were ranged from 0.01 to 1.00 mg/kg, the average fortified recoveries were in the range of 70.7 to 96.0% and the relative standard deviations were 1.2-6.4%. The limits of detection(LOD) for these pesticides were in the range of 0.12 to 1.4 μg/kg, while limits of quantification(LOQ) were in the range of 0.4 to 4.9 μg/kg. [Conclusions] The method is rapid and simple with high sensitivity and good reproducibility, which is suitable for determination of spirotetramat and its 4 metabolites in citrus and soil.

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