Food safety: sample dispersion in analytical control of organochlorine pesticides (4,4’-Dichlorodiphenyltrichloroethane and its metabolites, (alpha-, beta-, and gamma-isomers of Hexachlorocyclohexane)

Introduction. In assessing the safety of food products, analytical control of pesticide residues is relevant not only for currently used preparations, but also for a number of persistent, toxic substances, the production and use of which is prohibited or restricted worldwide. Such substances include organochlorine pesticides (OCPs) – 4,4’Dichlorodiphenyldichloroethane (DDT) and its metabolites, Hexachlorocyclohexane (HCH) (alpha, beta and gamma isomers), which belong to the class of persistent organic pollutants (POPs) with high stability in the environment.

The aim of the study. To develop an economical and rapid method of matrix solid-phase dispersion in combination with gas chromatography-mass spectrometry (MSPD-GC-MS) for the determination of OCP content in a wide range of raw materials and food products of animal origin, as well as products with a predominant content of components of animal origin.

Materials and methods. According to the sample preparation procedure using the matrix solid-phase dispersion method, crushed and homogenized food samples were dispersed in the florisil sorbent. The OCPs were extracted from the resulting bulk mixture with a mixture of organic solvents, and then the extract was purified with concentrated sulfuric acid. The samples were analyzed using a gas chromatograph “Chromatec-Crystal 5000.2” (Russian Federation) with a mass spectrometric detector.

Results. A simple method for determining organochlorine pesticides in a wide range of animal products using MTFD-GC-MS has been developed. Using florisil as a dispersant and a mixture of hexane and dichloromethane (1:1, by volume) as an eluting solvent, and including an additional stage of sample treatment with concentrated sulfuric acid allows achieving a good extraction and purification effect. The linearity range of the calibration curves is 0.005–0.2 µg/ml. The lower limit of quantification for all substances is 0.01 mg/kg, the degree of extraction varied from 85 to 104% with a relative standard deviation (RSD) of 6–8% (n = 5).

Limitations. In the study same types of food products of animal origin were considered as objects of research.

Conclusion. The method is characterized by its speed, simplicity, sufficient sensitivity, good reproducibility, and accuracy. It is suitable for the analysis of large volumes and meets the technical requirements for the determination of residual quantities of OCPs in food products of animal origin with a lower limit of quantification of an individual substance of 0.01 ppm.

Compliance with ethical standards. The study does not require a biomedical ethics committee opinion.

Contribution:
Fedorova N.E., Dobreva N.I., Goryacheva L.V. – concept and design of the study;
Dobreva N.I., Suslova A.V. – collection and processing of material;
Fedorova N.E., Dobreva N.I., Bondareva L.G. – text writing, editing.
All authors are responsible for the integrity of all parts of the manuscript and approval of the manuscript final version.

Conflict of interest. The authors declare no conflict of interest.

Funding. The study had no sponsorship.

Received: April 29, 2025 / Revised: June 2, 2025 / Accepted: June 26, 2025 / Published: October 20, 2025

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