多壁碳纳米管滤过型净化-超高效液相色谱-串联质谱法测定香蕉中氟唑菌酰胺和吡唑醚菌酯残留  

Determination of Fluxapyroxad and Pyraclostrobin Residues in Banana by Ultra-high Performance Liquid Chromatography- Tandem Mass Spectrometry Coupled with Multiplug Filtration Clean up with Multiwalled Carbon Nanotubes

作　　者：乐渊[1] 刘春华[1] 尹桂豪[1] 王明月[1] LE Yuan;LIU Chunhua;YIN Guihao;WANG Mingyue(Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables,Analysis&Testing Center,Chinese Academy of Tropical Agricultural Sciences,Haikou 571101)

机构地区：[1]中国热带农业科学院分析测试中心,海南省热带果蔬产品质量安全重点实验室,海南海口571101

出　　处：《分析科学学报》2020年第6期874-878,共5页Journal of Analytical Science

基　　金：现代农业产业技术体系建设专项资金(No.CARS-31-13);中国热带农业科学院基本科研业务费专项资金(No.1630082020002)。

摘　　要：建立了一种同时测定香蕉中氟唑菌酰胺和吡唑醚菌酯2种杀菌剂残留的超高效液相色谱-串联质谱方法。香蕉样品用乙腈提取后,经多壁碳纳米管滤过型净化柱净化,超高效液相色谱-串联质谱测定。氟唑菌酰胺和吡唑醚菌酯的质量浓度在0.005~0.2 mg/L范围内线性良好,相关系数均大于0.99,定量限均为5μg/kg。2种杀菌剂在香蕉中3个添加水平下的平均回收率在74.7%~102%范围,相对标准偏差在0.1%~8.2%之间。与N-丙基乙二胺、十八烷基键合硅胶、石墨化炭黑等吸附剂相比,多壁碳纳米管滤过型净化柱具有更好的净化性能。该方法具有简便、准确度高、净化效果好等优点,适用于香蕉中氟唑菌酰胺和吡唑醚菌酯残留量的快速检测。A method based on ultra-high performance liquid chromatography coupled with tandem mass spectrometry(UPLC-MS/MS) was developed for the simultaneous determination of fluxapyroxad and pyraclostrobin residues in banana.The banana samples were extracted with acetonitrile and cleaned up with multiplug filtration using multiwalled carbon nanotubes,then determined by UPLC-MS/MS.Calibration curves exhibited good linearity over the concentration range from 0.005 to 0.2 mg/L,with the correlation coefficients above 0.99.The limits of quantitation for both fungicides were 5 μg/kg.Average recoveries of two fungicides spiked at three levels in banana ranged from 74.7% to 102%,with the relative standard deviations ranging from 0.1% to 8.2%.Compared with primary secondary amine sorbent,octadecyl silane sorbent and graphitized carbon black sorbent,the multiplug filtration cleanup column has better purification performance.The developed method is sensitive,accurate and with good purification effect.It can be applied to the rapid determination of fluxapyroxad and pyraclostrobin residues in banana.

关 键 词：氟唑菌酰胺 吡唑醚菌酯 多壁碳纳米管 超高效液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学]