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Multiclass Method for the Determination of Pesticide Residues in Oat Using Modified QuEChERS with Alternative Sorbent and Liquid Chromatography with Tandem Mass Spectrometry
Food Analytical Methods ( IF 2.6 ) Pub Date : 2019-09-10 , DOI: 10.1007/s12161-019-01641-1
Estéfani M. C. de Matos , Lucila C. Ribeiro , Osmar D. Prestes , José A. G. da Silva , Bruna S. de Farias , Luiz A. de A. Pinto , Renato Zanella

Many pesticides are used for pest control during oat production and storage, making necessary to employ multiclass methods for pesticide residue determination. In this work, an efficient QuEChERS method was established for multiresidue determination of 60 pesticides in oats by liquid chromatography with tandem mass spectrometry (LC-MS/MS). Different sorbents, such as chitosan, Forisil®, C18, PSA, Supel QuE Z-Sep+, and EMR-Lipid were evaluated for cleanup by dispersive solid-phase extraction (d-SPE). The original QuEChERS method had the best performance and the biosorbent chitosan presented similar results to the other conventional sorbents evaluated and being an efficient and low-cost biodegradable material was chosen for the cleanup step. The method presented adequate accuracy and precision using blank samples spiked between 5 and 100 μg kg−1, with recovery from 70 to 120% and RSD < 20% for all 60 pesticides and limits of quantification of 5 μg kg−1 for almost all studied pesticides, with exception of triflumizole for which was 10 μg kg−1. The method was successfully applied in real samples proven to be a good option for routine analysis. Oat samples presented residues of azoxystrobin, metalaxyl, and thiamethoxam.



中文翻译:

改进的QuEChERS替代吸附剂和液相色谱-串联质谱法测定燕麦中农药残留的多类方法

燕麦生产和储存过程中使用了许多农药来控制害虫,因此有必要采用多种方法测定农药残留量。在这项工作中,建立了一种高效的QuEChERS方法,通过液相色谱-串联质谱法(LC-MS / MS)对燕麦中的60种农药进行多残留测定。通过分散固相萃取(d-SPE)评估了壳聚糖,C18,PSA,Supel QuE Z-Sep +和EMR-Lipid等不同吸附剂的净化效果。最初的QuEChERS方法具有最佳的性能,生物吸附剂壳聚糖的效果与其他常规吸附剂相似,并且作为一种有效且低成本的可生物降解材料被选作净化步骤。使用加标5至100μgkg的空白样品,该方法具有足够的准确性和精密度。-1,具有从70至120%的回收率和RSD <所有60种杀虫剂和5μg公斤的定量限20%-1几乎所有研究的杀虫剂,具有氟菌唑的例外,其为10μg千克-1。该方法已成功应用于实际样品中,被证明是常规分析的不错选择。燕麦样品中存在嘧菌酯,甲霜灵和噻虫嗪的残留物。

更新日期:2019-09-10
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