Determination of Pesticide Residues in Whole Wheat Flour Using Modified QuEChERS and LC–MS/MS

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• 作者：Aline B. Bordin ; Luciane Minetto ; Iraja do Nascimento Filho…
• 关键词：QuEChERS ; Pesticides ; Validation ; Whole eheat flour ; LC–MS/MS
• 刊名：Food Analytical Methods
• 出版年：2017
• 出版时间：January 2017
• 年：2017
• 卷：10
• 期：1
• 页码：1-9
• 全文大小：
• 刊物类别：Chemistry and Materials Science
• 刊物主题：Food Science; Chemistry/Food Science, general; Microbiology; Analytical Chemistry;
• 出版者：Springer US
• ISSN：1936-976X
• 卷排序：10

文摘

Pesticides in food are a major issue due to their intensive use in agriculture. Thus, an appropriate control of their residues in food samples should be done. In this study, a multiresidue method for the quantification of 37 pesticides in whole wheat flour was developed and validated. The modified QuEChERS (without cleanup) procedure followed by ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC–MS/MS) was used for analysis. The method was validated according to the European Union SANCO/12,571/ 2013 guidelines and Brazilian Manual of Analytical Quality Assurance. The following parameters were evaluated on the method validation: linearity, limit of detention, limit of quantification, matrix effect, precision, accuracy evaluating the percentage of recovery at three different spike levels, and robustness. Acceptable values were obtained. The linear range used was 1–200 μg kg−1, resulting to r2 of >0.99. The recovery was satisfactory with 70 and 120 % and RSD of <20 % for most compounds. Assessing the samples collected in the south Brazil region, some pesticide residues were detected in whole wheat flour (carbendazim, chlorpyrifos, deltamethrin, imidacloprid, malathion, pendimethalin, pirimiphos-methyl, triamedifom, and triadimenol). The applicability of this analytical approach was confirmed by successful determination of pesticides in whole wheat flour, a complex matrix.