Chromatographia

, Volume 63, Issue 1–2, pp 45–51 | Cite as

Determination of Aldehydes and Ketones in Fuel Ethanol by High-Performance Liquid Chromatography with Electrochemical Detection

  • A. A. Saczk
  • L. L. Okumura
  • M. F. de Oliveira
  • M. V. B. Zanoni
  • N. R. Stradiotto
Article

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 × 10−3 mol L−1 (80:20 v/v) and a flow-rate of 1.1mL min−1 . 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 mL−1, with detection limits of 1.7 to 2.0 ng mL−1 and quantification limits from 5.0 to 6.2 ng mL−1, using injection volume of 20 μL. The proposed methodology was simple, low time-consuming (15 min/analysis) and presented analytical recovery higher than 95%.

Keywords

Column liquid chromatography Electrochemical detection Aldehydes and ketones in fuel ethanol Dinitrophenylhydrazones 

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Copyright information

© Friedr. Vieweg & Sohn/GWV Fachverlage GmbH 2006

Authors and Affiliations

  • A. A. Saczk
    • 1
  • L. L. Okumura
    • 1
  • M. F. de Oliveira
    • 1
  • M. V. B. Zanoni
    • 1
  • N. R. Stradiotto
    • 1
  1. 1.UNESP – Instituto de QuímicaAraraquaraBrazil

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