Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, 23071, Jaén, Spain.
Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, 23071, Jaén, Spain.
J Chromatogr A. 2018 Aug 10;1562:27-35. doi: 10.1016/j.chroma.2018.05.053. Epub 2018 May 28.
In this article, a nanoflow liquid chromatography system coupled to high resolution mass spectrometry (nanoflow LC/ESI Q-Orbitrap-MS) has been applied for the development of a multiresidue pesticide method for the determination of 162 multiclass pesticides in olive oil samples. Due to the relatively high lipid content of the raw QuEChERS acetonitrile extracts obtained from this type of fatty vegetable samples, a dispersive solid phase extraction (dSPE) sorbent proposed to retain both fatty acids and triglycerides, namely Enhanced Matrix Removal-Lipid (EMR-Lipid) has been implemented as additional cleanup step. The analytical performances of the proposed method were evaluated,achieving recoveries in the range 75-119% with relative standard deviations lower than 19% (n = 6). The dSPE sorbent allowed the removal of most coextracted interferences without a significant loss of analytes. Matrix effects were also evaluated, showing a negligible effect for most of the compounds tested, when a dilution factor of 50 was applied. Notably, despite the use of relatively high dilution factors (e.g. 1:50) to minimize matrix effects, the lowest concentration levels detected with this method - in the low μg kg range - are well below the corresponding maximum residue levels established by the current European legislation.
本文采用纳流液相色谱-电喷雾串联四极杆轨道阱高分辨质谱联用仪（nanoflow LC/ESI Q-Orbitrap-MS），建立了橄榄油样品中 162 种多类农药残留的多残留检测方法。由于从这种高脂肪蔬菜样品的 QuEChERS 乙腈提取物中得到的原始提取物中含有相对较高的脂肪含量，因此采用了一种称为增强基质去除-脂类（EMR-Lipid）的分散固相萃取（dSPE）吸附剂作为额外的净化步骤，以保留脂肪酸和甘油三酯。评估了所提出方法的分析性能，在 75-119%的范围内获得了回收率，相对标准偏差低于 19%（n=6）。dSPE 吸附剂允许去除大多数共提取的干扰物，而不会显著损失分析物。还评估了基质效应，当应用 50 倍稀释因子时，发现大多数测试化合物的基质效应可忽略不计。值得注意的是，尽管使用了相对较高的稀释因子（例如 1:50）来最小化基质效应，但该方法检测到的最低浓度水平-在低μg/kg范围内-远低于现行欧洲法规规定的相应最大残留限量。
