中文摘要：本文开发了一个基于QuEChERS的高效样本处理方法和超高效液相色谱-质谱法的特异性检测器的检测方法，可用于检测蜂花粉中七种新烟碱类杀虫剂（啶虫脒、噻虫胺、呋虫胺、吡虫啉、烯啶虫胺、噻虫啉和噻虫嗪）残留。所有情况下，平均回收率均在91%-105%之间，没有发现任何基质效应。该方法的特异性好，线性范围为LODs-500μg/kg、精密度和准确性高，相对标准差和相对误差值均小于8%，检测限范围为0.6μg/kg-1.3μg/kg，定量限范围为2.1μg/kg-4.0μg/kg，应用该方法对西班牙不同地区市售蜂花粉样本中烟碱类杀虫剂残留进行了检测。
外文摘要：In this study, a new method has been developed to determine seven neonicotinoid insecticides (acetamiprid, clothianidin, dinotefuran, imidacloprid, nitenpyram, thiacloprid and thiamethoxam) in bee pollen using ultra-high performance liquid chromatography coupled to a selective MS detector (qTOF). An efficient sample treatment involving an optimized quick, easy, cheap, effective, rugged and safe method was proposed. In all cases, average analyte recoveries were between 91 and 105%, and no matrix effect was observed. Chromatographic analysis (6.5 min) was performed on a core-shell technology based column (Kinetex (R) R EVO C-18, 50x2.1 mm, 1.7 mu m, 100 angstrom). The mobile phase consisted of 0.1% formic acid in water and 0.1% of formic acid in ACN, with a flow rate of 0.3 mL/min in gradient elution mode. The fully validated method was selective, linear from LOQ to 500 mu g/kg, precise and accurate; relative standard deviation and relative error values were below 8%. Low limits LODs and LOQs were obtained, ranging from 0.6 to 1.3 mu g/kg (LODs) and 2.1 to 4.0 mu g/kg (LOQs). The method was applied to neonicotinoid analysis in several commercial bee pollen samples from different Spanish regions.
 
外文关键词：Bee pollen, Insecticides, Mass spectrometry, Neonicotinoids, Ultra-high performance liquid chromatography
作者：Valverde, Silvia; Luis Bernal, Jose; Teresa Martin, Maria; Jesus Nozal, Maria; Bernal, Jose
作者单位：Univ Valladolid, Analyt Chem Grp, IU CINQUIMA, E-47011 Valladolid, Spain.
期刊名称：ELECTROPHORESIS
期刊影响因子：2.482
出版年份：2016
出版刊次：10
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