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Determination of pesticides in edible oils by liquid chromatography-tandem mass spectrometry employing new generation materials for dispersive solid phase extraction clean-up

机译:液相色谱-串联质谱法测定食用油中的农药,采用新一代材料进行分散固相萃取净化

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The goal of this work was to evaluate the efficiency of several sorbents on removal fats from edible oils (olive, soya and sunflower) during the clean-up step for posterior determination of 165 pesticides by UHPLC-QqQ-MS/MS system. The extraction procedure employed in this work was the citrate version of QuEChERS method followed by a step of freezing out with dry ice and clean-up evaluation using i) PSA with magnesium sulfate (d-SPE); ii) magnesium sulfate and Z-sep sorbent (d-SPE); iii) Z-sep (column SPE) and iv) Agilent Bond Elut QuEChERS Enhanced Matrix Removal-Lipid (EMR-Lipid). After evaluation of the recovery results at 10, 20 and 50 mu g kg(-1), the EMR-Lipid showed important advantages comparing to the other sorbents evaluated, such as better recovery rates and RSD%. The method was validated at the three concentrations described above. Analytical curves linearity was evaluated by spiking blank oil samples at 10, 20, 50, 100 and 500 mu g kg(-1). The method demonstrated good recoveries values between the acceptable range of 70-120% and RSD% < 20 for most of evaluated pesticides. In order to evaluate the performance of the method, this same procedure was employed to other oils such as soya and sunflower with very good results. (C) 2016 Elsevier B.V. All rights reserved.
机译:这项工作的目的是评估在通过UHPLC-QqQ-MS / MS系统后部测定165种农药的净化步骤中,几种吸附剂对从食用油(橄榄油,大豆和向日葵)中去除脂肪的效率。这项工作采用的萃取程序是柠檬酸形式的QuEChERS方法,然后进行干冰冷冻,并使用i)带有硫酸镁(d-SPE)的PSA进行净化评估。 ii)硫酸镁和Z-sep吸附剂(d-SPE); iii)Z-sep(柱SPE)和iv)Agilent Bond Elut QuEChERS增强型脂质去除脂质(EMR-Lipid)。在评估了10、20和50μg kg(-1)的回收率结果后,与其他评估的吸附剂相比,EMR-Lipid显示出重要的优势,例如更好的回收率和RSD%。该方法在上述三种浓度下均得到验证。通过在10、20、50、100和500μg kg(-1)处添加空白油样品来评估分析曲线的线性度。该方法对大多数评估农药显示出在70-120%的可接受范围内且RSD%<20的良好回收率值。为了评估该方法的性能,对其他油(例如大豆油和向日葵油)使用了相同的步骤,效果非常好。 (C)2016 Elsevier B.V.保留所有权利。

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