Method of determining of polybrominated diphenyl ethers in fish and fish products by the method of liquid chromatography

The aim of the work was to develop a methodology for determining of polybrominated diphenyl ethers (PBDE) in fish and fish products for the control of impurities content in the food and environmental objects in general. The conditions of chromatography (temperature conditions, the impact of the speed and magnitude of dividing of the gas-carrier stream using a HP-1 capillary columns, the DB-5, HP-50 +, DB-1;) and lipids destructive and non-destructive cleaning methods of extract during the determination of PBDEs. The method of determination of 2,2,4,4-Tetrabromodiphenyl ether (BDE-47), 2,2,4,4,5-pentabromodiphenyl ether (BDE-99) and decabromodiphenyl ether (BDE-209) in fish and fish products by the liquid chromatography with electron detector was suggested. The method of PBDE is based on the extraction of samples with hexane-acetone (3:1), purification of the extract with concentrated sulfuric acid (phase ratio hexane-sulfuric acid - 5:1). The second purification step is carried out by using solid phase extraction cartridges «SiOH-H2SO4/SA» and hexane as the eluent. Gas chromatographic analysis of the determination of BDE-47 and BDE-99 is carried out on low-polar capillary column DB-5 (30 m x0.25 mm x0.25 mum) with the programming of the column temperature. In determining the BDE-209 a DB-1 nonpolar capillary column was used (15 m x 0.25 mm x 0.1 mum) with the column temperature programming. Calculation of the content of BDE-47 and BDE-99 is carried out with the internal standard (2,2, 3,4,4-pentabromodiphenyl ether (BDE-85)), BDE-209 by absolute calibration. In determining the BDE-209 the calibration matrix was used. The range of concentrations of the calibration solutions for the determination of BDE-47 and BDE-99 is 0.005-0.05 g/cm3, for BDE-209 0.05-0.3 g/cm3. The technique allows the measurement of BDE-47 and BDE-99 in the range of 0.0002-0.05 mg/kg of the product concerned; BDE-209 - in the range of 0.002-0.3 mg/kg. The metrological characteristics of the method were calculated.