title: Evaluation of solid-phase microextraction methods for determination of trace concentration aldehydes in aqueous solution.
abstract: A method for trace analysis of a wide range of aldehydes (saturated/unsaturated aliphatic, aromatic aldehydes, including hydroxylated species, and dialdehydes) in an aqueous solution was optimized. An evaluation of three solid-phase microextraction (SPME) techniques (headspace, liquid-phase, and on-fiber derivatization) with o-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) aldehyde derivatization was performed focusing on the optimization of the main extraction parameters (temperature and time). The optimized method employed the liquid-phase SPME (D-L-SPME) of derivatized aldehydes at 80 degrees C for 30 min. Limits of detection (LODs) using this optimal method were in the range of 0.1-4.4 microg/L for the majority of aliphatic (saturated, unsaturated), aromatic aldehydes and dialdehydes. Formaldehyde LODs and those of some hydroxylated aromatic aldehydes were between 32 and 55 microg/L. Headspace SPME using an on-fiber derivatization generally showed a lower sensitivity and several compounds were not detected. Another technique, the optimized headspace SPME of aldehydes derivatized in aqueous solution, was not as sensitive as D-L-SPME for hydroxylated aromatic aldehydes. The developed method was used to analyze aqueous particulate matter extracts; this method achieved higher sensitivities than those obtained with US Environmental Protection Agency (EPA) Method 556.
authors.affiliation: Chemistry Department, University of North Dakota, 151 Cornell Street, Grand Forks, ND 58202, USA.
authors.forename: Josef
authors.initials: J
authors.lastname: Beránek
authors.forename: Alena
authors.initials: A
authors.lastname: Kubátová
mesh_terms: D000447:Aldehydes / Q000032:analysis* / Q000302:isolation & purification; D008401:Gas Chromatography-Mass Spectrometry; D015203:Reproducibility of Results; D052617:Solid Phase Microextraction / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000302:isolation & purification
chemical_list: D000447:Aldehydes; D014874:Water Pollutants, Chemical