The invention relates to the complex approach of determination of the environmental pollution by persistent organic pollutants from a single extraction procedure using samples of biological origin and could be used for monitoring of the environment, particularly for monitoring of persistent contamination of surface waters using biological objects such as fish as an indicator. The proposed complex approach for determination of persistent organic pollutants involves the quantitative extraction from samples of biological origin using the mixture of organic solvents; segregation of the extract into two parts; stage clean-up of the first part of the extract from the high-molecular compounds using gel permeation chromatography and acid modified silica gel column chromatography; separation of fraction containing polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs), polybrominated dibenzo-p-dioxins and dibenzofurans (PBDD/Fs) and mixed bromo-, chloro-substituted dibenzo-p-dioxins and dibenzofurans (PXDD/Fs) from fraction containing polybrominated diphenyl ethers (PBDEs), mixed bromo-, chloro-substituted biphenyls (PXBs) and polychlorinated biphenyls (PCBs) by means of quantitative fractionation of the purified first part of the extract using three stage column chromatography with magnesium sulfate, activated carbon and aluminum oxide; separation of persistent organic pollutants from the non-ortho substituted PCB and PXB group by means of fractionation of the first part of the extract containing PBDEs, PXBs and PCBs using activated carbon column chromatography; analysis of PCDD/F, PBDD/F, PXDD/F, PBDE, PXB and PCB group compounds using gas chromatography – high resolution mass spectrometry; destructive separation of high molecular weight compounds from the second part and clean-up of the remaining fraction which contains hexabromocyclododecane compounds (HBCDs) by means of magnesium silicate column chromatography; analysis of HBCD compounds using ultra high performance liquid chromatography – high resolution mass spectrometry.
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