Department of Analytical Chemistry, Faculty of Chemistry, Gdańsk University of Technology (GUT), Narutowicza 11/12 street, 80-233 Gdańsk, Poland.
Molecules. 2018 Oct 9;23(10):2582. doi: 10.3390/molecules23102582.
Developed and validated analytical methods for the determination of a wide spectrum of pesticide residues in honey and honeybee samples after the modification of QuEChERS extraction in combination with gas chromatography⁻tandem quadrupole mass spectrometry (GC-MS/MS) and liquid chromatography⁻tandem quadrupole mass spectrometry (LC-MS/MS) were discussed and compared. The developed methods were evaluated regarding the utilized equipment and reagents using Eco-Scale and compared in terms of extraction time, accuracy, precision, sensitivity and versatility, with similar procedures. The results proved that the QuEChERS protocol in combination with LC and GC techniques fulfills the requirements of green analytical chemistry, so it can be used as a tool in environmental monitoring. The recovery was 85⁻116% for honey and 85.5⁻103.5% for honeybee samples. The developed methods were successfully applied in monitoring real samples collected from three districts of Pomerania in Poland. Analysis of real samples revealed the presence of the following pesticides: bifenthrin, fenpyroximate, methidathione, spinosad, thiamethoxam, triazophos, metconazole and cypermethrin at levels higher than the MRLs established by the EU.
讨论并比较了 QuEChERS 提取方法改良后,结合气相色谱-串联四极杆质谱(GC-MS/MS)和液相色谱-串联四极杆质谱(LC-MS/MS),用于测定蜂蜜和蜜蜂样品中多种农药残留的分析方法的开发和验证。 利用生态规模(Eco-Scale)评估了所使用设备和试剂的开发方法,并与类似程序相比,在提取时间、准确性、精密度、灵敏度和通用性方面进行了比较。 结果证明,结合 LC 和 GC 技术的 QuEChERS 方案符合绿色分析化学的要求,因此可作为环境监测的工具。 蜂蜜和蜜蜂样品的回收率分别为 85⁻116%和 85.5⁻103.5%。 所开发的方法成功应用于监测从波兰波美拉尼亚三个地区采集的实际样品。 对实际样品的分析表明,存在以下农药:联苯菊酯、唑虫酰胺、甲硫威、多杀菌素、噻虫嗪、三唑磷、咪鲜胺和氯氰菊酯,其水平高于欧盟设定的 MRL。