| Article ID | Journal | Published Year | Pages | File Type |
|---|---|---|---|---|
| 1243026 | Talanta | 2010 | 10 Pages |
Simultaneous analysis of 24 carbonyl compounds (alkanals, unsaturated, dicarbonylic and aromatic aldehydes and ketones) derivatized with 2,4-dinitrophenylhydrazine and 16 polycyclic aromatic hydrocarbons (PAHs) using a photodiode-array (PDA) and a fluorescence (FL) detector in series is proposed.The separation is carried out with a reversed-phase column and gradient elution using four solvents (acetonitrile, water, tetrahydrofuran and methanol) in less than 35 min. Several critical pairs of carbonyl compounds with 3 and 4 carbon atoms and different functional groups, isomers of tolualdehyde, aromatic and aliphatic aldehydes were conditional on the gradient elution. Common pre-treatment for two groups of compounds consists in a step of extraction and derivatization in aqueous medium and a further clean-up using a polymeric phase SPE and concentration in a mixture of dichloromethane:methanol. A pre-concentration factor of 50 was achieved by this procedure. Acetone and formaldehyde blanks were minimized and remain controlled with a specific cleaning of glass material and washing the SPE cartridge.The limits of detection (LOD) ranged from 0.006 to 0.18 ng mL−1 for PAHs and from 2.4 to 10.1 ng mL−1 for carbonyl compounds and method precision was ≤15% for all analysed compounds. Recoveries were within the range of 95–104% for PAHs except for more volatile compounds (acenaphthene and fluorene) and within the range of 72–113% for carbonyl compounds. The method was applied in water-soluble fraction of PM10 (atmospheric particulate matter with an aerodynamic diameter less than 10 μm) and the spectral contrast technique was used in the identification of carbonyl compounds.
