Affiliation:
1. Lipetsk State Technical University
Abstract
Purpose of research. The aim of the work is to optimize the conditions for gas chromatographic determination of a mixture of eight organochlorine pesticides: aldrin, hexachlorobenzene, heptachlor, α-hexachlorocyclohexane, γ-hexachlorocyclohexane, dichlorodiphenyltrichloromethylmethane, dichlorodiphenyldichloroethane and dichlorodiphenyldichloroethylene.Methods. For chromatographic studies of organochlorine pesticides we used a Shimadzu GC-2010Plus gas chromatograph (Shimadzu, Japan) equipped with an automatic equilibrium vapor sample dispenser NT200N, electron-capture detector based on 63Ni and quartz capillary nonpolar column "Chromatek" SPB-5 (30 m, 0.32 mm, film thickness on the basis of phenyl(5%) and dimethyl(95%) polysiloxanes 0.5 μm) with an operating temperature range of 60°C 320/340°C. The chromatograms were processed in the application LabSolutions GPC.Results. On the basis of experimentally obtained data the optimal conditions for gas chromatographic determination and separation of eight-component mixture of organochlorine pesticides were selected, namely: the value of mobile phase flow division 1:10, carrier gas flow rate – 1.0 ml/min, two-stage temperature programmable column mode from 160 to 240°C with the rate of increase of 5°C/min. The metrological characteristics of the analysis and validation of the results of the proposed technique with the method of high-performance liquid chromatography were evaluated. Good reproducibility of chromatography results with the possibility of detection of organochlorine pesticides at the level of 10-6 – 10-5 μg/cm3 was proved. Application of Fisher's test has shown absence of significant differences in reproducibility of sampled populations the investigated methods of chromatographic analysis of COPCs are equally accurate. Extraction sample preparation of samples of real objects was proposed, the calculated extraction degrees >84% allow to recommend the technique for quantitative determination of analytes.Conclusion. The method of gas chromatographic analysis was tested for determination of organochlorine pesticides in samples of drinking water and baby puree (Russia) by additive method. Exceeding the norms of residual contents of organochlorine pesticides in the samples of the food products under study was not detected.
Publisher
Southwest State University
Reference20 articles.
1. Lavrukhina O. I., Amelin V. G., Kish L. K., Tretyakov A. V., Lavrukhin D. K. Opredelenie ostatochnykh kolichestv pestitsidov v ob"ektakh okruzhayushchei sredy i pishchevykh produktakh [Determination of pesticide residues in environmental objects and food]. Khimicheskaya bezopasnost' = Chemical Safety, 2022, vol. 6, no. 2, рр. 81–116. https://doi.org/10.25514/CHS.2022.2.23006
2. Tian D., Mao H., Lu H., Zheng Y., Peng C., Hou S. Novel two-tiered approach of ecological risk assessment for pesticide mixtures based on joint effects. Chemosphere, 2018, vol. 192, pp. 362–371. https://doi.org/10.1016/j.chemosphere.2017.11.001
3. Galiulin R. V., Galiulina R. A., Horobrykh R. R., Bashkin V. N. Risk sovremennogo zagryazneniya rechnykh vod pestitsidami DDT i GKhTsG [Risk of modern river water pollution by pesticides ddt and ghcg]. Problemy analiza riska = Problems of risk analysis, 2019, vol. 16, no. 5, pp. 62–69. https://doi.org/10.32686/1812-5220-2019-16-5-62-69
4. Rahman M. Monitoring of pesticide residues from fish feed, fish and vegetables in Bangladesh by GC-MS using the QuEChERS method. Heliyon, 2021, vol. 7(3), pp. 1–8. https://doi.org/10.1016/j.heliyon.2021.e06390
5. Zhen X., Liu L., Wang X., Zhong G., Tang J. Fates and ecological effects of current-use pesticides (CUPs) in a typical river-estuarine system of Laizhou Bay. North China. Environmental Pollution, 2019, vol. 252, pp. 573–579. https://doi.org/10.1016/j.envpol.2019.05.141