Abstract
Nowadays, highly polar pesticides are not included in multiresidue methods due to their physico-chemical characteristics and therefore, specific analytical methodologies are required for their analysis. Laboratories are still looking for a pluri-residue method that encompasses the largest number of polar pesticides. The aim of this work was the simultaneous determination of ethephon, 2-hydroxyethylphosphonic acid (HEPA), fosetyl aluminum, glyphosate, aminomethylphosphonic acid (AMPA), N-acetyl-glyphosate and N-acetyl-AMPA in tomatoes, oranges, aubergines and grapes. For that purpose, an ultra high performance liquid chromatography (UHPLC) coupled to a high resolution single mass spectrometer Orbitrap-MS were used. Different stationary phases were evaluated for chromatographic separation, and among them, the stationary phase Torus DEA provided the best separation of the selected compounds. The QuPPe method was used for the extraction of the analytes, but slight modifications were needed depending on the matrix. The developed method was validated, observing matrix effect in all matrices. Intra- and inter-day precision were estimated, and relative standard deviation were lower than 19%. Recoveries were satisfactory, and mean values ranged from 70% to 110%. Limits of quantification were between 25 and 100 µg kg−1. Finally, the analytical method was applied to different fruits and vegetables (oranges, tomatoes, aubergines and grapes).
Highlights
High polar pesticides have different physico-chemical characteristics compared with other pesticides, and they are not included in multiresidue methods, and a pluri-residue method is required for their simultaneous analysis [1]
In the last few years, the most common strategy is based on using new stationary phases, due to the fact that derivatization increases the manipulation of the sample, increasing errors associated to this step
The aim of this study was the development of a pluri-residue method for the simultaneous determination of polar pesticides and metabolites
Summary
High polar pesticides have different physico-chemical characteristics compared with other pesticides, and they are not included in multiresidue methods, and a pluri-residue method is required for their simultaneous analysis [1]. In the last few years, the most common strategy is based on using new stationary phases, due to the fact that derivatization increases the manipulation of the sample, increasing errors associated to this step. The European Reference Laboratory (EURL, EU Reference Laboratory) developed a generic method, named Quick Polar Pesticides Methods (QuPPe) [7], based on the extraction of polar pesticides. Foods 2020, 9, 553 from the sample with acidified methanol and liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). This was used for the determination of polar pesticides in different food [8]
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