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.
Departamento de Química Analítica, Facultade de Ciencias, Universidade da Coruña, Campus da Zapateira, E-15071 A Coruña, Spain.
M C
MC
Prieto-Blanco
Y
Y
Moliner-Martínez
P
P
López-Mahía
P
P
Campíns-Falcó
D000447:Aldehydes / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods; D007659:Ketones / Q000032:analysis*; D057230:Limit of Detection; D013058:Mass Spectrometry; D052638:Particulate Matter / Q000737:chemistry*; D010659:Phenylhydrazines / Q000737:chemistry; D052617:Solid Phase Microextraction; D014874:Water Pollutants, Chemical / Q000032:analysis*
D000447:Aldehydes; D007659:Ketones; D052638:Particulate Matter; D010659:Phenylhydrazines; D014874:Water Pollutants, Chemical; C004787:2,4-dinitrophenylhydrazine
Capillary LC–mass spectrometry; Carbonyl compounds; In-tube solid phase microextraction; PM(2.5); Water