Determination of pesticide residues by chromatographic methods for food safety

Abstract

The paper presents the methodology of preparation of samples of oilseeds, lettuce, apples for research by chromatographic control of xenobiotics of the following chemical groups of pesticides: benzimidazole derivatives, anilinopyrimidine derivatives, bipyridylium derivatives. The implementation of the following processes is considered: homogenization of the sample, purification of the extract by solid-phase or liquid-liquid extraction, obtaining a plant extract, obtaining an extract of analytes. For fine-grained homogenized samples of sunflower seeds, the optimal ratio of raw material -extragent is 1:20, for pasty homogenized samples of apple fruit - 1:10, for liquid samples of homogenized lettuce - 1: 5. Analysis of the distribution of xenobiotics in the system octane/water, the dipole moment of solvents allowed to determine the extractants that are able to dissolve and remove xenobiotics from raw materials. It was found that a mixture of acetonitrile and methanol (4: 1) should be used to remove benzimidazole derivatives and anilinopyrimidine derivatives, bipyridylium derivatives are best extracted with methanolic trifluoroacetic acid (9.5: 0.5). Quantitative analysis of xenobiotics content in extracts obtained from samples artificially enriched with xenobiotics was performed. The most complete xenobiotics were removed from samples of plant products containing traces of fat. The most difficult process of sample preparation is the process of obtaining sunflower seed extract. The content of xenobiotics in extracts obtained from samples artificially enriched in analytes is influenced by the temperature at which the process takes place and the duration of extraction. Based on the chemical composition of the sample matrix and the list of analytes, the conditions of the variable component of the methodology are proposed: obtaining plant extract under the action of selective solvents, homogenized raw material-solvent with constant stirring of the extraction system at 180-200 rpm, or under the action of ultrasonic vibrations with a frequency of 37 kHz from 4°C to 25°C for 5-25 minutes. The control of the qualitative and quantitative composition of the studied plant extracts and analyte extracts was investigated by the methods of high-performance liquid and gas chromatography (liquid and gas) with mass-selective detectors.