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Identification and quantification of PAH in bitumen by GC-Ion-Trap MS and HPLC-fluorescent detectors
Polycyclic Aromatic Compounds
Bitumen is a complex product with a large matrix of heavy aliphatic/naphthenic/aromatic hydrocarbons as well as a large number of isomeric compounds such as polycyclic aromatic compounds (PACs). Some PACs and derivatives are known to have a mutagenic and carcinogenic activity, and there is no generally satisfactory clean-up method for separating PACs from this very complex hydrocarbon matrix. Moreover, from an analytical point of view, the isomeric compounds usually co-elute in the same gas chromatography (GC) retention range, GC being one of the most widely used techniques in this area. However, the use of a suitable clean-up procedure for isolating the aromatic fractions, combined with two selective detection techniques such as mass spectrometry (GC-Ion Trap MS) and HPLC-Fluorescent detector (HPLC-FL), is expected to provide an effective tool for accurately determining certain PAC species in bitumen. In this paper we compare two quantitative extractions to analyse the 16 PAHs that occur in bitumen according to the US EPA reference list. Two clean-up protocols are assessed and compared by using both GC-Ion Trap MS and HPLC-FL chromatographic/detection techniques. The first extraction method combines well-established and proven clean-up operations with an automatic fractionation by semi-preparative HPLC (certification test program for PAHs in sewage sludge, in creosote-contaminated soil and in harbour sediment organised by the Community Bureau of Reference, BCR). The second method uses a multiple step-by-step liquid/liquid and liquid/solid extraction clean-up procedure. After the bitumen extracts are cleaned up, only the use of both GC-MS & HPLC-FL can provide reliable results. The more sensitive FL provides enhanced fluorescent selectivity signals that facilitate identification of PAH compounds. However, for their quantification, the capillary GC-ion trap mass spectrometric technique is preferred because of the insufficient resolution of the HPLC column and the possible quenching or co-elution effect of matrix compounds. Both detection techniques are regarded as complementary. [Authors]
Polycyclic Hydrocarbons, Aromatic , Gas Chromatography, Mass Spectrometry , Spectrometry, Mass, Electrospray Ionization
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