Simultaneous determination of carbonyl compounds and polycyclic aromatic hydrocarbons in atmospheric particulate matter by liquid chromatography–diode array detection–fluorescence detection

• Published in: Talanta (Oxford) 2010-03, Vol.80 (5), p.2083-2092
• Main Authors: Prieto-Blanco, M.C., Iglesias, M. Piñeiro, López-Mahía, P., Lorenzo, S. Muniategui, Rodríguez, D. Prada
• Format: Article
• Language: English
• Subjects: Aldehydes - analysis; Analytical chemistry; Carbonyl compounds; Carcinogens - analysis; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, High Pressure Liquid - instrumentation; Chromatography, High Pressure Liquid - methods; Environmental Monitoring - instrumentation; Environmental Monitoring - legislation & jurisprudence; Environmental Monitoring - methods; Exact sciences and technology; Fluorescence; HPLC–PDA–FL; Ketones - analysis; Limit of Detection; Other chromatographic methods; Particulate Matter - analysis; PM 10; Polycyclic aromatic hydrocarbons; Polycyclic Aromatic Hydrocarbons - analysis; Simultaneous analysis; Water-soluble organic compounds (WSOC)
• ISSN: 0039-9140; 1873-3573
• DOI: 10.1016/j.talanta.2009.11.009

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 PM 10 (atmospheric particulate matter with an aerodynamic diameter less than 10 μm) and the spectral contrast technique was used in the identification of carbonyl compounds.