Uclés Ana, Herrera López Sonia, Dolores Hernando Maria, Rosal Roberto, Ferrer Carmen, Fernández-Alba Amadeo R
Agrifood Campus of International Excellence (ceiA3), European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, University of Almeria, Spain.
National Institute for Agriculture and Food Research and Technology, INIA, 28040 Madrid, Spain.
Talanta. 2015 Nov 1;144:51-61. doi: 10.1016/j.talanta.2015.05.055. Epub 2015 May 30.
The use of yttria-stabilized zirconium dioxide nanoparticles as d-SPE clean-up sorbent for a rapid and sensitive liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) method for the determination of post-harvest fungicides (carbaryl, carbendazim, chlorpropham, diphenylamine, ethoxyquin, flutriafol, imazalil, iprodione, methomyl, myclobutanil, pirimiphos-methyl, prochloraz, pyrimethanil, thiabendazole, thiophanate-methyl and tolclofos-methyl) in orange and pear samples has been evaluated and validated. The sample preparation was a modification of the QuEChERS extraction method using yttria-stabilized zirconium dioxide and multi-walled carbon nanotubes (MWCNTs) nanoparticles as the solid phase extraction (d-SPE) clean-up sorbents prior to injecting the ten-fold diluted extracts into the LC system. By using the yttria-stabilized zirconium dioxide extraction method, more recoveries in the 70-120% range were obtained - thus this method was used for the validation. Quantification was carried out using a matrix-matched calibration curve which was linear in the 1-500 µg kg(-1) range for almost all the pesticides studied. The validated limit of quantification was 10 µg kg(-1) for most of the studied compounds, except chlorpropham, ethoxyquin and thiophanate-methyl. Pesticide recoveries at the 10 and 100 µg kg(-1) concentration levels were satisfactory, with values between 77% and 120% and relative standard deviations (RSD) lower than 10% (n=5). The developed method was applied for the determination of selected fungicides in 20 real orange and pear samples. Four different pesticide residues were detected in 10 of these commodities; 20% of the samples contained pesticide residues at a quantifiable level (equal to or above the LOQs) for at least one pesticide residue. The most frequently-detected pesticide residues were: carbendazim, thiabendazole and imazalil-all were below the MRL. The highest concentration found was imazalil at 1175 µg kg(-1) in a pear sample.
已对使用氧化钇稳定的二氧化锆纳米颗粒作为分散固相萃取（d-SPE）净化吸附剂的方法进行了评估和验证，该方法用于通过快速灵敏的液相色谱-电喷雾电离-串联质谱法（LC-ESI-MS/MS）测定橙子和梨样品中的采后杀菌剂（西维因、多菌灵、氯苯胺灵、二苯胺、乙氧喹、粉唑醇、抑霉唑、异菌脲、灭多威、腈菌唑、甲基嘧啶磷、咪鲜胺、嘧霉胺、噻菌灵、甲基硫菌灵和甲基立枯磷）。样品制备是对QuEChERS萃取方法的改进，在将稀释十倍的提取物注入LC系统之前，使用氧化钇稳定的二氧化锆和多壁碳纳米管（MWCNTs）纳米颗粒作为固相萃取（d-SPE）净化吸附剂。通过使用氧化钇稳定的二氧化锆萃取方法，获得了70%-120%范围内更高的回收率，因此该方法用于验证。使用基质匹配校准曲线进行定量，对于几乎所有研究的农药，该校准曲线在1-500 μg kg⁻¹范围内呈线性。除了氯苯胺灵、乙氧喹和甲基硫菌灵外，大多数研究化合物的验证定量限为10 μg kg⁻¹。在10和100 μg kg⁻¹浓度水平下，农药回收率令人满意，值在77%至120%之间，相对标准偏差（RSD）低于10%（n = 5）。所开发的方法用于测定20个实际橙子和梨样品中的选定杀菌剂。在其中10种商品中检测到四种不同的农药残留；20%的样品含有至少一种农药残留的可量化水平（等于或高于定量限）。最常检测到的农药残留是：多菌灵、噻菌灵和抑霉唑，均低于最大残留限量。在一个梨样品中发现的最高浓度是抑霉唑，为1175 μg kg⁻¹。
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