| 超高效液相色谱-串联质谱法同时检测柑橘样品中氟吡呋喃酮及其代谢物残留 |
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| 基金项目:湖南省高校产业化培育项目（13CY030）；湖南省高校创新平台开放基金项目（15K066）；湖南人文科技学院产学研合作引导项目（2013CXY04）；湖南省2017年研究生创新科研项目（CX2017B779） |
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| 中文摘要:采用超高液相色谱-串联质谱（UPLC-MS/MS） 技术建立了同时检测柑橘全果、橘肉及橘皮中氟吡呋喃酮及其代谢物二氟乙酸（DFA）、6-氯烟酸（6-CNA）和二氟乙氨基呋喃酮（DFEAF）残留的分析方法。样品经乙腈提取，分散固相萃取（PSA）净化，采用电喷雾电离（ ESI+/ESI-） 快速正负切换模式，多反应监测模式（MRM） 扫描，外标法定量。结果表明，氟吡呋喃酮及其代谢物在1~500 μg/L范围内线性关系良好，相关系数为0.997 9~0.999 6,检出限为0001 mg/L；在0.05、0.3、2 mg/kg加标水平下，柑橘全果、果肉中氟吡呋喃酮及其代谢物的回收率为71.9%~106%，相对标准偏差（RSD）为0.8%~9.1%；在0.1、0.3、3 mg/kg加标水平下，柑橘果皮的回收率为77.9%~100%，RSD为1.2%~6.5%。氟吡呋喃酮及其代谢物在柑橘全果、橘肉和橘皮中的定量下限（LOQ）分别为0.05、0.05、0.1 mg/kg。该方法操作简便、快速准确，适于柑橘基质中氟吡呋喃酮及其代谢物残留量的快速检测。 |
| 中文关键词:农药残留 氟吡呋喃酮 代谢产物 柑橘 超高效液相色谱-串联质谱（UPLC-MS/MS） |
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| Simultaneous Determination of Flupyradifurone and Its Metabolites in Citrus Samples Using Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| Abstract:An analytical method was developed for the simultaneous detection of flupyradifurone and its three metabolites ie.difluoroacetic acid（DFA），6-chloronicotinic acid（6-CNA） and difluoroethylaminofuranone（DFEA） in citruses by ultrahigh performance liquid chromatography tandem mass spectrometry（UPLC-MS/MS）.Citrus samples were extracted with acetonitrile，and cleaned up by dispersive solid phase extraction（PSA）.The analytes were detected in multiple reaction monitoring（MRM） mode under alternate positive/negative electrospray ionization（ESI+/ESI- ） mode，and quantified by the external standard method.The results showed that there were good linearities for flupyradifurone and its metabolites in their respective concentration ranges with correlation coefficients of 0.997 9-0.999 6.The limits of detection were 0.001 mg/L.The average recoveries for the analytes in the whole citrus fruit and fruit pulp at spiked levels of 0.05，0.3 and 2 mg/kg ranged from 71.9%to 106%with relative standard deviations（RSDs） of 0.8%-9.1%.The average recoveries of the analytes in citrus fruit peel at spiked levels of 0.1，0.3 and 3 mg/kg ranged from 77.9%to 100%with relative standard deviations（RSDs） of 1.2%-6.5%.The limits of quantitation（LOQs） for flupyradifurone and its metabolites in the whole citrus fruit，fruit pulp and peel were 0.05，0.05 and 0.1 mg/kg，respectively.The method is simple，stable，rapid and sensitive，and is suitable for the determination of flupyradifurone and its metabolites in citrus samples. |
| Key Words:pesticide residue flupyradifurone metabolites citrus ultrahigh performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） |
| 引用本文：李双双,欧晓明,金晨钟,晏姣,张贵群,梁骥,梁贵平.超高效液相色谱-串联质谱法同时检测柑橘样品中氟吡呋喃酮及其代谢物残留[J].分析测试学报,2018,37(11):1354-1358. |
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