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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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作者单位
李双双,欧晓明,金晨钟,晏姣,张贵群,梁骥,梁贵平 1.湖南人文科技学院农药无害化应用重点实验室/湖南省农田杂草防控技术与应用协同创新中心2.湖南化工研究院国家农药创制工程技术研究中心3.湖南加法检测有限公司 
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)
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0001 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)
 
Simultaneous Determination of Flupyradifurone and Its Metabolites in Citrus Samples Using Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry
Abstract:An analytical method was developed for the simultaneous detection of flupyradifurone and its three metabolites ie.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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