Bernardi Gabrieli, Kemmerich Magali, Adaime Martha B, Prestes Osmar D, Zanella Renato
Laboratório de Análises de Resíduos de Pesticidas (LARP), Departamento de Química, Universidade Federal de Santa Maria, 97105-900 Santa Maria-RS, Brazil.
Anal Methods. 2020 Jun 4;12(21):2682-2692. doi: 10.1039/d0ay00744g.
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 μg L-1. Trueness results, obtained by recovery assays at the spike levels 10, 20, 50 and 100 μg 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 μg L-1.
开发并验证了一种用于葡萄酒样品中97种农药多残留测定的小型化样品制备方法。所提出的萃取程序基于QuEChERS乙酸盐方法,并采用分散固相萃取(d-SPE)进行净化步骤。采用超高效液相色谱-串联质谱(UHPLC-MS/MS)进行测定。对萃取和净化步骤进行了评估,以获得所选农药的最佳条件。样品制备步骤的小型化减少了样品和化学品的消耗。方法定量限在10至20μg L-1之间。通过在10、20、50和100μg L-1加标水平下的回收率测定获得的准确度结果范围为70%至120%,相对标准偏差(RSD)表示的精密度≤20%。该方法成功应用于葡萄酒样品分析,发现不同农药的浓度在14至55μg L-1之间。