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采用多壁碳纳米管分散固相萃取和超高效液相色谱-串联质谱法同时测定植物和动物源性样品中氟吡菌胺及其主要代谢物残留量。

Simultaneous determination of cyflumetofen and its main metabolite residues in samples of plant and animal origin using multi-walled carbon nanotubes in dispersive solid-phase extraction and ultrahigh performance liquid chromatography-tandem mass spectrometry.

机构信息

State Key Laboratory for Biology of Plant Diseases and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, China.

出版信息

J Chromatogr A. 2013 Jul 26;1300:95-103. doi: 10.1016/j.chroma.2013.05.052. Epub 2013 May 28.

Abstract

A rapid and effective method for the simultaneous determination of cyflumetofen and its main metabolite residues in samples of plant and animal origin (tomato, apple, eggplant, soybean, green tea, fish, and pork liver) was developed using ultrahigh performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Samples were extracted with acetonitrile and cleaned-up with multi-walled carbon nanotubes (MWCNTs). The determination of the presence of target compounds was achieved in less than 4.0min using an electrospray ionization source in the positive mode (ESI+) for cyflumetofen and 2-(trifluoromethyl) benzamide (B-3) and the negative mode (ESI-) for α,α,α-trifluoro-o-toluic acid (B-1). The entire method was validated by evaluating the repeatability, linearity, precision, trueness, and matrix effect. Average recoveries of the analytes were in the range of 79.3-117.6% with relative standard deviation values below 7.6%. Limits of quantification (LOQs) ranged from 0.7 to 9.8μgkg(-1), which were lower than the maximum residue limits (MRLs) for the cyflumetofen found in foods in Japan.

摘要

建立了一种超高效液相色谱-串联质谱法(UPLC-MS/MS),用于快速有效地检测植物和动物源性样品(番茄、苹果、茄子、大豆、绿茶、鱼和猪肝)中的氟吡菌酰胺及其主要代谢物残留。样品用乙腈提取,用多壁碳纳米管(MWCNTs)净化。使用电喷雾电离源在正模式(ESI+)下对氟吡菌酰胺和 2-(三氟甲基)苯甲酰胺(B-3)进行检测,在负模式(ESI-)下对α,α,α-三氟-o-甲苯酸(B-1)进行检测,目标化合物的存在可在不到 4.0min 内确定。通过评估重复性、线性、精密度、准确度和基质效应来验证整个方法。分析物的平均回收率在 79.3-117.6%之间,相对标准偏差值低于 7.6%。定量限(LOQs)范围为 0.7-9.8μgkg(-1),低于日本食品中氟吡菌酰胺的最大残留限量(MRLs)。

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