Determination of carbonyl compounds in particulate matter PM2.5 by in-tube solid-phase microextraction coupled to capillary liquid chromatography/mass spectrometry

In this paper, a new procedure based on in-tube solid phase microextraction (IT-SPME)-capillary liquid chromatography hyphenated to mass spectrometry detection by using microelectrospray ionisation (CapLC–MS), has been reported. The device was proposed to quantify 12 carbonyl compounds (10 aliphatic aldehydes, an unsaturated aldehyde and a ketone) derivatized with 2,4-dinitrophenylhidrazine (DNPH) reagent in aqueous extracts of PM2.5. This methodology involves the on-line preconcentration of DNPH-carbonyl compounds derivatives coupled to the CapLC–MS system, efficiently providing appropriate sensitivity for the determination of the target analytes. Detection limits for the analytes ranged between 0.9 and 8.2 ng L−1. These values represent a remarkable improvement over the existing methods since PM2.5 analysis can be carried out avoiding off-line preconcentration steps. The procedure is also proved useful for analysing water samples. Under the optimised conditions, IT-SPME-CapLC–MS shows satisfactory recovery values (80–90%) for spiked samples.