Plant and Soil Science

Methodological approaches to sample preparation for xenobiotic content analysis

Nataliia Tereshchenko, Olena Khyzhan, Kateryna Nesterova
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Abstract

The aim of the article was to improve sample preparation protocols and chromatographic analysis conditions for the determination of selected xenobiotics in agricultural products. To achieve this goal, a method of artificial fortification of homogenised samples of sunflower seeds, corn kernels, lettuce leaves, and apples with model xenobiotics of different classes was used, followed by extraction with organic solvents using a modified QuEChERS approach and quantitative analysis. For the effective extraction of acetochlor and prometryn from lettuce leaves and apples, which are characterised by a high water content, an optimal raw material-to-extractant ratio of 1:3-1:5 was found. In the case of corn kernels, which have a structure containing a negligible amount of lipids, the extraction was performed with a ratio of 1:10. The greatest difficulties were observed during the processing of sunflower seeds, where a three-phase system formed due to the high fat content, complicating the mass transfer of analytes. Nevertheless, the use of acetonitrile as an extractant in a 1:17-1:20 ratio allowed for high extraction rates of the target xenobiotics to be achieved. For the extraction of benomyl and cyprodinil, a mixture of acetonitrile and methanol in a 4:1 ratio was used, which ensured effective transfer of the specified analytes in all studied matrices. Specifically, in lettuce and apple samples, the extraction rates for both substances exceeded 96%, which indicated good solubility in the mixture used and a low matrix effect. For diquat, a bipyridylium compound with a pronounced ionic nature, the best results were obtained using a solution of trifluoroacetic acid in methanol in a 9.5:0.5 ratio. This composition ensured stable extraction from all types of plant matrices, with maximum values in lettuce samples and minimum values in sunflower seeds (86%), which still meets modern requirements for analytical accuracy. In the case of corn kernel samples, the extraction level for all substances was 88-92%, which indicated satisfactory extractability in cereal matrices. The lowest extraction values were recorded for sunflower seeds; however, even under these conditions, the extraction remained within the 80-86% range, which is acceptable according to international standards for pesticide analysis quality control. The results of the chromatographic analysis confirmed the high reproducibility and sensitivity of the method

Keywords

high-performance liquid chromatography; gas chromatography with mass-selective detectors; extracts; pesticides; plant extracts

Suggested citation
Tereshchenko, N., Khyzhan, O., & Nesterova, K. (2025). Methodological approaches to sample preparation for xenobiotic content analysis. Plant and Soil Science, 16(3), 9-21. https://doi.org/10.31548/plant3.2025.09
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