Published: Journal of Chromatographic Science, ISSN 0021-9665 Volume 44, Number 6, July 2006, pp.347-353

HS–SPME Determination of Volatile Carbonyl and Carboxylic Compounds in Different Matrices

Elena E. Stashenko[1], Amanda L. Mora[2], Martha Cervantes[1], and Jairo R. Martínez[1]
[1]Laboratorio de Cromatografía-CIBIMOL, Escuela de Química, Facultad de Ciencias, Universidad Industrial de Santander, A.A. 678, Bucaramanga, Colombia and
[2]Escuela de Química, Universidad Nacional de Colombia, Sede Medellín, Colombia

Specific chromatographic methodologies are developed for the analysis of carboxylic acids (C2–C6, benzoic) and aldehydes (C2–C10) of low molecular weight in diverse matrices, such as air, automotive exhaust gases, human breath, and aqueous matrices. For carboxylic acids, the method is based on their reaction with pentafluorobenzyl bromide in aqueous solution, followed by the separation and identification of the resultant pentafluorobenzyl esters by means of headspace (HS)–solid-phase microextraction (SPME) combined with gas chromatography (GC) and electron capture detection (ECD). Detection limits in the µg/m3 range are reached, with relative standard deviation (RSD) less than 10% and linear response (R2 > 0.99) over two orders of magnitude. The analytical methodology for aldehydes is based on SPME with simultaneous derivatization of the analytes on the fiber, by reaction with pentafluorophenylhydrazine. The derivatization reagent is previously deposited on the SPME fiber, which is then exposed to the gaseous matrix or the HS of the sample solution. The pentafluorophenyl hydrazones formed on the fiber are analyzed selectively by means of GC–ECD, with detection limits in the ng/m3 range, RSD less than 10%, and linear response (R2 > 0.99) over two orders of magnitude.

Reproduction of editorial content of this journal is prohibited without publisher’s permission.