Characterization of chemical interferences in the determination of unsaturated aldehydes using aromatic hydrazine reagents and liquid chromatography

Rasmus Schulte-Ladbeck; Roger Lindahl; Jan-Olof Levin; Uwe Karst

doi:10.1039/B101354H

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Rasmus Schulte-Ladbeck,^a Roger Lindahl,^b Jan-Olof Levin^b and Uwe Karst*^a

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* Corresponding authors

^a Westfälische Wilhelms-Universität Münster, Anorganisch-Chemisches Institut, Abteilung Analytische Chemie, Wilhelm-Klemm-Str. 8, Münster, Germany

^b National Institute for Working Life, P.O. Box 7654, Umeå, Sweden

Abstract

A systematic investigation on interferences in the determination of unsaturated aldehydes and ketones using the 2,4-dinitrophenylhydrazine (DNPH) method is described. Acrolein, crotonaldehyde, methacrolein and 1-buten-3-one are derivatized with DNPH in the presence of an acidic catalyst to form the respective hydrazones. The unstable hydrazones react with excess reagent to form adducts. These are identified by high-performance liquid chromatography (HPLC)-mass spectrometry and spectroscopic techniques after cryogenic fraction collection of the adducts. The quantification of the unsaturated carbonyls with the DNPH method remains difficult. N-Methyl-4-hydrazino-7-nitrobenzofurazan (MNBDH) was used as an alternative reagent for this purpose. As with DNPH, the formation of a side product is observed. In contrast to DNPH, the alteration of the pH immediately after sampling leads to only one reaction product, which is stable and storable in solution at 4 °C for 2 days.

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Article information

DOI: https://doi.org/10.1039/B101354H
Article type: Paper
Submitted: 12 Feb 2001
Accepted: 18 Apr 2001
First published: 09 May 2001

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J. Environ. Monit., 2001,3, 306-310

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