A new analytical method using high performance liquid chromatography-diode array detector (HPLC-DAD) was developed for the analysis of 18 benzimidazoles and their metabolites in milk. Samples were extracted with acetonitrile and n-hexane...

Glyphosate is the most used herbicide in agriculture. Its major metabolite is AMPA (aminomethylphosphonic acid), but N-acetyl-AMPA and N-acetylglyphosate are also metabolites of interest. For risk assessment, a general residue definition was proposed as the sum of glyphosate, AMPA, N-acetyl-glyphosate and N-acetyl-AMPA, expressed as glyphosate. A confirmatory method for glyphosate in fat, liver and kidneys, as well as a confirmatory method for AMPA and N-acetyl-glyphosate in all matrices, are still missing. In this paper, we present a method for the quantitative determination of glyphosate residues and its metabolites AMPA, N-acetyl-AMPA and N-acetyl-glyphosate by liquid chromatography–mass spectrometry (LC-MS/MS) in adipose tissue, liver, eggs, milk and honey without derivatization. Different chromatographic columns were tested, with the Hypercarb column providing the best results. The analytes were eluted with mobile phases of acidified water with 1.2% formic acid and 0.5% formic acid in acetonitrile. Sample purification procedures were also optimized by varying the solvent extraction mixtures (water, methanol and mixture ψ (methanol, water) = 1:1, each with the addition of 1% formic acid (v/v)), using different sorbents in solid phase extraction (SPE) (polymeric cationic (PCX) and anionic (PAX)) and using dispersive solid phase extraction (dSPE) (C18 and PSA) by modifying the extraction procedures. Finally, the analytes were extracted from the samples with 1% formic acid in water (v/v). Milk and adipose tissue were purified by the addition of dichloromethane, while liver and egg samples were purified by SPE with a mixed cation exchange sorbent and ultrafiltration with cut-off filters. The proposed analytical procedures were validated according to SANTE/11312/2021 guidelines: linearity, limits of quantification, precision and accuracy were determined for all matrices. The limits of quantification (LOQs) ranged from 0.025 to 0.2 mg kg⁻¹. Precision, expressed as relative standard deviation, was <20%, while accuracy, expressed as analytical recovery, ranged from 70% to 120%. During method validation, the measurement uncertainty was estimated to be <50% for all analytes. Good validation parameters according to the SANTE document were achieved for all analytes. Therefore, the method can be considered reliable and sensitive enough for routine monitoring of polar pesticides. The application of the accredited method in routine analysis will provide data that are useful for the re-evaluation of risk assessment studies in foods of animal origin.

Polycyclic aromatic hydrocarbons (PAHs) are organic compounds consisting of carbon and hydrogen atoms, with more than two fused benzene rings. PAHs are associated with risks to human health, particularly carcinogenesis. One exposure route is the ingestion of contaminated food, which can result from high-temperature preparation and processing (such as grilling, smoking, toasting, frying, and deep-frying), as well as from PAHs present in soil, air, and water due to environmental pollution, including incomplete combustion or pyrolysis of organic matter during industrial processing and motor vehicle exhaust. Deposition of PAHs from the air leads to their entry into soil, which is their main route into the environment – sediments and water. Analytical methods for determining PAHs in environmental samples include extraction, purification, and detection techniques. Sample preparation is a crucial step in the analysis of PAHs, especially in complex food matrices that require efficient extraction and clean-up procedures to isolate PAHs from co-extracted matrix components. This review provides an overview of the available literature – from sample preparation procedures, extraction and clean-up methods, to instrumental analytical techniques in various matrices, including soil, water (wastewater, drinking water, surface water), and food of animal origin (egg, milk) – thus offering a comprehensive summary in one place. The paper also reviews the occurrence of PAHs in different types of matrices in the context of legislation.