Peter Haglund

Isolation of toxic polychlorinated biphenyls by electron donor—acceptor high-performance liquid chromatography on a 2-(1-prenyl)ethyldimethylsilylated silica column

A rapid and simple liquid chromatographic method for the isolation of toxic planar polychlorinated biphenyls from their formulations by electron donor-acceptor high-performance liquid chromatography using a 2-(1-pyrenyl)ethyldimethylsilylated silica column is described. The separation takes less than 15 min and a complete analysis, including quantitation by gas chromatography-mass spectrometry or gas chromatography with electron-capture detection, may be completed in 60 min. Retention data for 105 individual polychlorinated biphenyl congeners are presented and the retention behaviour, as well as the mechanisms of separation, are discussed.

Analysis of halogenated polycyclic aromatic hydrocarbons in urban air, snow and automobile exhaust

Abstract Urban air, snow and automobile exhaust samples were extensively cleaned up by open column liquid chromatography. The appropriate fractions were analysed for halogenated polycyclic aromatic hydrocarbons (XPAH) by gas chromatography/negative chemical ionization mass spectrometry (GC/NCIMS). XPAH were found in all three sample types. A urban air sample was found to contain chlorinated pyrenes, fluoranthenes and benzopyrene and brominated pyrenes and fluoranthenes. Furthermore, the concentration of 1-chloropyrene in that air sample was estimated to be 10 pg/m3. XPAH were also found in snow samples taken in the vicinity of a motor-way. Ethylene dibromide and ethylene dichloride, are probably the source of the halogen atoms in the XPAH detected in car exhaust.

Isolation of mono- and non-ortho polychlorinated biphenyls from biological samples by electron-donor acceptor high performance liquid chromatography using a 2-(1-pyrenyl)ethyldimethylsilylated silica column

Abstract A method for the analysis of both mono- and non-ortho polychlorinated biphenyls (PCBs) in biological tissue samples is described. The method includes solvent extraction, sulfuric acid/n-hexane partitioning, gel permeation chromatography and finally electron-donor acceptor high performance liquid chromatography using a 2-(1-pyrenyl)ethyldimethylsilylated silica column (PYE column). The PYE column separates PCBs according to the number of chlorine atoms in the ortho positions. Gas chromatography/mass spectrometry (GC/MS) and GC/electron capture detection (GC/ECD) were used to analyze the non- and the mono-ortho PCB fractions, respectively. The method was found to give high recoveries and a low degree of discrimination between different PCB congeners.

Analysis of non-ortho polychlorinated biphenyls and polychlorinated naphthalenes in Swedish dioxin survey samples

Abstract The coplanar (non-ortho) polychlorinated biphenyls (pPCB) 3,3′4,4′-tetrachlorobiphenyl (IUPAC 77), 3,3′4,4′5-pentachlorobiphenyl (IUPAC 126), 3,3′4,4′5,5′-hexachlorobiphenyl (IUPAC 169) and polychlorinated naphthalenes (PCN) were analyzed in biological and sediment samples. The predominant congeners found in biological samples were IUPAC 77, IUPAC 126, two early eluting pentachloronaphthalenes and one early eluting hexachloronaphthalene. Baltic herring show seasonal differences in pPCB and PCN levels. The lipid weight levels in cod muscle and liver are very similar despite differences in fat content. Pike and sediment from a PCB-contaminated river contain very high levels of pPCB and PCN but have PCDD/F levels that are not unusually high. There are differences in the levels and isomer pattern between the sediment and pike indicating metabolism and bioaccumulation. There is a significant correlation between total and planar PCB content in herring and cod samples. The toxic potential of pPCB in most of the fish samples expressed as TCDD toxic equivalents more than equals that of PCDD/F.

Analysis of polybrominated dioxins and furans in vehicle exhaust

Abstract The exhaust from three vehicles (two cars, fueled with leaded and unleaded gasoline, respectively, and a heavy duty diesel truck) were investigated for the presence of polybrominated dibenzo-p-dioxins and dibenzofurans (PBDD/F). Both the particulate and the gas phase were sampled. The corresponding particulate and gas phase extracts were combined and then cleaned up by liquid chromatography using different adsorbents, and by liquid/liquid partition between sulfuric acid and n-hexane. Finally, the samples were analyzed by gas chromatography/negative chemical ionization mass spectrometry (GC/NCIMS). DBDF, TrBDD/F, TeBDD/F and PeBDF were found in the exhausts from the car fueled with leaded gasoline, and TrBDF and TeBDF were found in the exhausts from the car fueled with unleaded gasoline. The amounts of PBDD/F emitted from the former car were found to be about two order of magnitude higher than from the latter. However, PBDD/F were not detected in the diesel exhaust. Dibromoethane is probably the major source of the bromine atoms in the PBDD/F detected in exhaust from cars fueled with leaded gasoline.

Analysis of bromo-, chloro- and mixed bromochloro-dibenzo-p-dioxins and dibenzofurans in salmon, osprey and human milk

Muscle samples from salmon and osprey as well as human mothers milk were solvent extracted and cleaned up extensively by chemical digestion followed by chromatography on various adsorbents. Appropriate fractions were analyzed for brominated, chlorinated, and bromochlorinated dibenzo-p-dioxins and dibenzofurans (PBDD/F, PCDD/F and PXDD/F, respectively) by high-resolution gas chromatography/high-resolution mass spectrometry. PCDD/F were found in all samples analyzed, however in no cases were PBDD/F or PXDD/F detected despite low limits of detection, < 1 ppt in most cases.