中文摘要：对食品农药残留和污染物检测技术的评估，一直是人们比较关注的问题。本文应用2×3因子设计建立了一种LC-MS/MS技术检测小麦多种农药残留的分析方法。结果显示，该方法对所有化合物的线性拟合度R2大于0.99，基体效应在3%-97%之间，在10和100μg/kg加标水平下的回收率在70%-120%之间且相对标准差为20%，检测限为3.3-6.7μg/kg，定量限10-20μg/kg，扩展不确定性在15%-32%之间。该方法的检测效果达到了同时检测小麦样本中42种农药残留的水准。
外文摘要：The evaluation of analytical methods for determining the level of residues and contaminants in food samples is a continuing need. To improve this evaluation, it is necessary to investigate different extraction procedures and conditions. A 2(3) factorial design was applied to establish an analytical method for determining pesticide residues in wheat by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Factors that influence the recovery of compounds, such as agitation and different processes of partition and cleanup, were investigated. Extracts were analyzed by LC-MS/MS with electrospray ionization in a triple quadrupole system. The use of ultrasonic agitation in the extraction step, deep freezing for the partition step, and C18 cleanup provided significantly better recoveries for most of the compounds evaluated. Assessment of each factor as well as interactions between factors allowed for a more effective evaluation of the parameters involved in the development of analytical methods. The validation results were satisfactory, since the method presented linearity (r (2)) > 0.99 for all compounds, the matrix effect ranged from 3 to 97 % and was corrected by matrix-matched standards, and recoveries ranged from 70 to 120 % with RSD a parts per thousand currency sign20 % for the spike levels of 10 and 100 mu g kg(-1). The method limit of detection and limit of quantification ranged from 3.3 to 6.7 mu g kg(-1) and from 10 to 20 mu g kg(-1), respectively, and the expanded uncertainty ranged from 15 to 32 %. The proposed method met the criteria for determination of 42 pesticides in wheat samples and was successfully tested in real samples.
外文关键词：Pesticides；Cereal；Sample preparation；Design of experiments；LC-MS/MS
作者：Maria T. Friedrich；Manoel L. Martins；Osmar D. Prestes
作者单位：Centro de Pesquisa em Alimentao, Universidade de Passo Fundo, CEP 99001-970 Passo Fundo, RS, Brazil
期刊名称：Food Analytical Methods
期刊影响因子：2.167
出版年份：2016
出版刊次：2
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