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采用 QuEChERS-气相色谱串联质谱法分析干果果中的多种类农药。

Analysis of multiclass pesticides in dried fruits using QuEChERS-gas chromatography tandem mass spectrometry.

机构信息

Departamento de Ciencias Básicas, Facultad de Ingeniería, Universidad EAN. Calle 79 n° 11-45, Bogotá D.C., Colombia; Departamento de Química, Unidad Departamental de Química Analítica, Facultad de Ciencias, Universidad de La Laguna (ULL). Avda. Astrofísico Francisco Sánchez, s/n°. 38206 San Cristóbal de La Laguna, Spain.

Departamento de Ciencias Básicas, Facultad de Ingeniería, Universidad EAN. Calle 79 n° 11-45, Bogotá D.C., Colombia.

出版信息

Food Chem. 2019 Nov 1;297:124961. doi: 10.1016/j.foodchem.2019.124961. Epub 2019 Jun 8.

Abstract

In this work, three versions of the QuEChERS method (original, AOAC 2007.01 and CEN 15662) were evaluated for the extraction of 38 multiclass pesticides from a mixture of five dried fruits: (strawberry, blackberry, passion fruit, pineapple and grapes) prior to their gas chromatography tandem mass spectrometry analysis. Among them, the AOAC 2007.01 method provided the best results in terms of lower amount of matrix co-extractives, matrix effect, extraction efficiency and precision. Its application to the analysis of the same pesticides in the individual dried fruits provided good recovery (between 70 and 120%) and relative standard deviation values (<20%) for most pesticides at three spiked levels. Matrix effect assessment revealed the necessity of taking into account such effect. Matrix-matched calibration data were also satisfactory for all analytes and matrices being the R ≥ 0.9900 and the lowest calibration level 5 µg/kg, which is lower than the agreed limit set at 10 µg/kg for monitoring purposes in food applications. Three samples of each type were also analysed, finding residues of metalaxyl, chlorpyrifos and iprodione in some of them.

摘要

在这项工作中,评估了三种 QuEChERS 方法(原始方法、AOAC 2007.01 和 CEN 15662),用于从五种干水果(草莓、黑莓、百香果、菠萝和葡萄)混合物中提取 38 种多类农药,然后进行气相色谱串联质谱分析。其中,AOAC 2007.01 方法在基质共提物、基质效应、提取效率和精密度方面表现出更好的效果。该方法应用于单独的干水果中相同农药的分析,对于大多数农药,在三个加标水平下,均获得了良好的回收率(70%至 120%之间)和相对标准偏差值(<20%)。基质效应评估表明有必要考虑这种效应。对于所有分析物和基质,基质匹配校准数据也令人满意,相关系数(R)≥0.9900,最低校准水平为 5µg/kg,低于食品应用中监测目的设定的 10µg/kg 商定限量。还对每种类型的三个样本进行了分析,发现其中一些样本中存在金属axyl、毒死蜱和异丙菌胺的残留。

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