In situ continuous derivatization/pre-concentration of carbonyl compounds with 2,4-dinitrophenylhydrazine in aqueous samples by solid-phase extraction Application to liquid chromatography determination of aldehydes

A rapid and straightforward continuous solid-phase extraction system has been developed for in situ derivatization and pre-concentration of carbonyl compounds in aqueous samples Initially 2,4-dinitrophenylhydrazine, the derivatizing agent, was adsorbed on a C-18 mini-column and then 15-ml of sample were continuously aspirated into the flow system, where the derivatization and pre-concentration of the analytes (low-molecular mass aldehydes) were performed simultaneously. Following elution, 20 mu l of the extract were injected into a LC-DAD system. in which hydrazones were successfully separated in 12 min on a RP-C-18 column using a linear gradient mobile phase of acetonitrile-water of 60-100% acetonitrile for 8 min. flowing at 0.5 ml/min. The whole analytical process can be accomplished within ca. 35 min. Under optimum conditions, limits of detection were obtained between 0.3 and 1.0 mu g/l and RSDs (inter-clay precision) from 1.2 to 4.6%. Finally, some applications on water samples are presented with recoveries ranged from 95.8 to 99.4%. (C) 2008 Elsevier B.V. All rights reserved.