Development of controls method for the isomers of polycyclic aromatic hydrocarbons in vegetable oils

L. O. Nesterova, N. Y. Hrybova, O. I. Khyzhan, V. O. Ushkalov


Actuality. In the conditions of intensive development of the oil-extracting, refining and petrochemical industries, as a result of processes of incomplete combustion of organic compounds, an enormous amount of pollution is released into the environment. For monitoring of the safety of plant material before 2015, as a marker of contamination was used the most toxic representative of a group of polycyclic aromatic hydrocarbons (PAHs), carcinogen - benzo(a)pyrene. In May 2016 the Order of the Ministry of Health of Ukraine No. 368  was came into  force, according to which three compounds of the PAHs group are regulated in food products: benzo(a)pyrene (BaP), benzo(b)fluorene (BbF), benzo(a)anthracene (BaA). In the EU, according to Commission Regulation (EC) No 835/2011, four PAHs are regulated in food products: benzo(a)pyrene, benzo(b)fluorene, benzo(a)anthracene and chrysene. Benzo(e)pyrene (BeP) is the benzo(a)pyrene isomer but the BeP does not have carcinogenic activity and does not require the regulations. The purpose of the research. The development and testing of the laboratory control method, which will allow to provide analysis of complex mixtures: benzo(a)pyrene, benzo(b)fluorene, benzo(a)anthracene, chrysene. The materials and methods for investigation. The next appropriate fractions of the whole materials were used: sunflower oil-crude and refined sunflower oil. The solutions of analytical standards of PAHs were dissolved in the acetonitrile and in the isopropanol.
Sorbents (activated carbon, solid-phase extraction cartridges and solid-phase extraction cartridges). The solvents for "chromatography": acetone, methanol, isopropanol, acetonitrile, deionized water, orthophosphoric acid. Work with samples was carried out in accordance with the following methods: standardized, tested and developed earlier in the Ukrainian laboratory of quality and safety of agricultural products of the National University of Life and Environmental Sciences of Ukraine (ULQSAP AP of NUBiPU) Measurements were carried out by liquid and gas chromatography with mass-selective detectors (HPLC/MS/MS, GC/MS). The results and discussion. The process of chromatographic separation of a mixture of polycyclic aromatic hydrocarbons containing isomers with different carcinogenic activity were investigated. Optimal conditions for measuring the content of four regulated oils and fatty products of compounds have been established: benzo(a)pyrene, benzo(b)fluorene, benzo(a)anthracene and chrysene. The method which was proposed has passed the validation procedure, the method was designed for measuring the content of polycyclic aromatic hydrocarbons, which are normalizing in Ukraine and the EU. The method can be applied in laboratory control of refining efficiency, for identify the conformity of products to sanitary and hygienic standards. Conclusions. The optimal conditions of chromatographic analysis of polycyclic aromatic hydrocarbons, allowing to carry out laboratory control of mixtures of PAHs which are normalized: (BaP), (BbF), (BaA), chrysene.

Ключові слова

polycyclic aromatic hydrocarbons, benzo(a)pyrene, vegetable oil, laboratory control, high performance liquid chromatography, refining

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