Abstract
A new methodology was developed for analysis of aldehydes and ketones in fuel ethanol by high-performance liquid chromatography (HPLC) coupled to electrochemical detection. The electrochemical oxidation of 5-hydroxymethylfurfural, 2-furfuraldehyde, butyraldehyde, acetone and methyl ethyl ketone derivatized with 2,4-dinitrophenylhydrazine (DNPH) at glassy carbon electrode present a well defined wave at +0.94 V; +0.99 V; +1.29 V; +1.15 V and +1.18 V, respectively which are the basis for its determination on electrochemical detector. The carbonyl compounds derivatized were separated by a reverse-phase column under isocratic conditions with a mobile phase containing a binary mixture of methanol / LiClO4(aq) at a concentration of 1.0 Ă 10â3 mol Lâ1 (80:20 v/v) and a flow-rate of 1.1mL minâ1 . The optimum potential for the electrochemical detection of aldehydes-DNPH and ketones-DNPH was +1.0 V vs. Ag/AgCl. The analytical curve of aldehydes-DNPH and ketones-DNPH presented linearity over the range 5.0 to 400.0 ng mLâ1, with detection limits of 1.7 to 2.0 ng mLâ1 and quantification limits from 5.0 to 6.2 ng mLâ1, using injection volume of 20 ÎŒL. The proposed methodology was simple, low time-consuming (15 min/analysis) and presented analytical recovery higher than 95%.
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