Simultaneous determination of carbonyl compounds and polycyclic aromatic hydrocarbons in atmospheric particulate matter by liquid chromatography-diode array detection-fluorescence detection.
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 <or=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 microm) and the spectral contrast technique was used in the identification of carbonyl compounds.
Prieto-Blanco
M C
MC
Department of Analytical Chemistry, Faculty of Sciences, Campus A Zapateira, E-15071 A Coruña, Spain.
Iglesias
M Piñeiro
MP
López-Mahía
P
P
Lorenzo
S Muniategui
SM
Rodríguez
D Prada
DP
D000447:Aldehydes / Q000032:analysis*; D002273:Carcinogens / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods*; D004784:Environmental Monitoring / Q000295:instrumentation / Q000331:legislation & jurisprudence / Q000379:methods; D005453:Fluorescence; D007659:Ketones / Q000032:analysis*; D057230:Limit of Detection; D052638:Particulate Matter / Q000032:analysis*; D011084:Polycyclic Aromatic Hydrocarbons / Q000032:analysis*
D000447:Aldehydes; D002273:Carcinogens; D007659:Ketones; D052638:Particulate Matter; D011084:Polycyclic Aromatic Hydrocarbons