Retrospective analysis of pesticide metabolites in urine using liquid chromatography coupled to high-resolution mass spectrometry

• A retrospective screening has been developed for pesticide metabolites in urine.
• A customised database of 263 pesticide metabolites was built for suspect analysis.
• 26 pesticide metabolites were identified in urine samples.
• 8 metabolites were confirmed at concentration from 0.79 to 141.04 ng mL−1.
• The urine samples were grouped according to their origin.

A comprehensive retrospective analysis of pesticide metabolites in urine was developed, using liquid chromatography coupled to Orbitrap high-resolution mass spectrometry (UHPLC-HRMS) that includes both post-run target (suspect screening) and non-target screening. An accurate-mass database comprising 263 pesticide metabolites was built and used for the post-run screening analysis. For non-target analysis, a “fragmentation-degradation” relationship strategy was selected. The proposed methodology was applied to 49 real urine samples from pregnant women. In the post-target analysis 26 pesticide metabolites were tentatively identified, 8 of which (2-diethylamino-6-methyl-pyrimidinol; 3-ketocarbofuran; 4,6-dimethoxy-2-pyrimidinamine; 4-hydroxy-2-isporopyl-6-methylpyrimidine; diethyl malate; diethyl maleate; N-(2-Ethyl-6-methylphenyl)-2-hydroxyacetamide and propachlor oxanilic acid ) were confirmed using analytical standards. Likewise, one unknown degradation product, methyl-N-phenylcarbamate was elucidated in the non-target screening. Finally, the real urine samples were grouped according to their origin applying a metabolomic approach.

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