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Miniaturized QuEChERS method for determination of 97 pesticide residues in wine by ultra-high performance liquid chromatography coupled with tandem mass spectrometry

机译:用超高效液相色谱法与串联质谱法一起测定红酒中97种农药残留的小型QueChers方法

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摘要

A miniaturized sample preparation method was developed and validated for the multiresidue determination of 97 pesticides in wine samples. The proposed extraction procedure is based on the QuEChERS acetate method with dispersive solid phase extraction (d-SPE) for the clean-up step. Ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS) was used for determination. The extraction and clean-up steps were evaluated to obtain the best conditions for the selected pesticides. Miniaturization of the sample preparation step provided a reduction in the consumption of samples and chemicals. The method limit of quantification was between 10 and 20 mu g L-1. Trueness results, obtained by recovery assays at the spike levels 10, 20, 50 and 100 mu g L-1, ranged from 70 to 120% with precision in terms of relative standard deviations (RSD) <= 20%. The method was successfully applied for the analysis of wine samples and different pesticides were found at concentrations from 14 to 55 mu g L-1.
机译:开发了一种小型化的样品制备方法,并验证了葡萄酒样品中97种农药的多途径测定。所提出的提取方法基于QueChers乙酸酯方法,用于清洁步骤的分散固相萃取(D-SPE)。用串联质谱(UHPLC-MS / MS)偶联的超高效液相色谱法测定。评价提取和清理步骤以获得所选农药的最佳条件。样品制备步骤的小型化提供了样品和化学品消耗的减少。定量的方法限制在10至20μgl-1之间。通过尖峰水平10,20,50和100μmg -1的回收测定获得的特征结果,在相对标准偏差(RSD)<= 20%方面,精度为70%至120%。该方法已成功应用于分析葡萄酒样品,并以14至55μg1-1的浓度发现不同的农药。

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  • 来源
    《Analytical methods》 |2020年第21期|共11页
  • 作者单位

    Univ Fed Santa Maria Dept Quim Lab Anal Residuos Pesticidas LARP BR-97105900 Santa Maria RS Brazil;

    Univ Fed Santa Maria Dept Quim Lab Anal Residuos Pesticidas LARP BR-97105900 Santa Maria RS Brazil;

    Univ Fed Santa Maria Dept Quim Lab Anal Residuos Pesticidas LARP BR-97105900 Santa Maria RS Brazil;

    Univ Fed Santa Maria Dept Quim Lab Anal Residuos Pesticidas LARP BR-97105900 Santa Maria RS Brazil;

    Univ Fed Santa Maria Dept Quim Lab Anal Residuos Pesticidas LARP BR-97105900 Santa Maria RS Brazil;

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  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 分析化学;
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