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2C - Biomarkers (TUP/110) Optimisation of procedure for determination of polycyclic aromatic hydrocarbons (PAHs) in bioindicators. Tomaniova, Monika1, Janska, Marie1, Kocourek, Vladimir 1, Hasjlova, Jana1, 1 Institute of Chemical Technology, Prague, Czech Republic ABSTRACT- Polycyclic aromatic hydrocarbons (PAHs) represent one of the most important group of environmental pollutants possessing carcinogenic/mutagenic potential. Analyses of various environmental matrices (sediments, soil, vegetation, atmosphere,...) are commonly carried out within many research studies and/or monitoring programs to assess the risk for exposed biota. Many data are also generated in order to control compliance to legislation limits. Generally, relevant matrices with certified concentrations of target analytes should be used to check trueness of results. Unfortunately, the availability of certified reference materials (CRMs) fitting to particular purpose is very limited. The aim of presented study was to develop and validate analytical procedure for determination of 16 priority polycyclic aromatic hydrocarbons (EPA list), together with their methylated derivatives and selected sulfur-containing heterocyclic aromatic hydrocarbons in several biotic matrices. The optimisation of procedure was focused on all its steps, i.e. extraction, clean-up and quantitation. The efficiency (expressed as recovery) of three alternative extraction procedures (sonication, Soxhlet and accelerated solvent extraction, ASE) employing several solvent mixtures was studied. Gel permeation chromatography (GPC) employing either Bio-Beads S-X3 or Pl rigid gel column was used for purification of crude extracts prior to determinative chromatographic step. Reversed phase high performance liquid chromatography with fluorimetric detection (HPLC-FLD) was applied for a routine identification and quantification of all the analytes involved in study. Gas chromatography with mass spectrometric detection (GC-MS) was used for the purpose of confirmation. The performance characteristics obtained by classic quadrupol analyzer were compared with those obtained by high resolution time of flight analyzer (TOF-MS). Standard uncertainties of each individual step were calculated, accuracy of HPLC-FLD and GC-MS procedures was critically assessed. This study was carried out within the project No. MSM 223300004 supported by the Ministry of Education and Youth of the Czech Republic. Key words: environmental pollutants, PAH's |
