Characterization of chemical interferences in the determination of unsaturated aldehydes using aromatic hydrazine reagents and liquid chromatography.
作者： Rasmus SchulteLadbeck , Roger Lindahl , JanOlof Levin , Uwe Karst
DOI: 10.1039/B101354H
关键词: Hydrazine 、 High-performance liquid chromatography 、 Crotonaldehyde 、 Chromatography 、 Acrolein 、 Chemistry 、 Reagent 、 Methacrolein 、 Mass spectrometry 、 Organic chemistry 、 Adduct
摘要: A systematic investigation on interferences in the determination of unsaturated aldehydes and ketones using 2,4-dinitrophenylhydrazine (DNPH) method is described. Acrolein, crotonaldehyde, methacrolein 1-buten-3-one are derivatized with DNPH presence an acidic catalyst to form respective hydrazones. The unstable hydrazones react excess reagent adducts. These identified by high-performance liquid chromatography (HPLC)-mass spectrometry spectroscopic techniques after cryogenic fraction collection quantification carbonyls remains difficult. N-Methyl-4-hydrazino-7-nitrobenzofurazan (MNBDH) was used as alternative for this purpose. As DNPH, formation a side product observed. In contrast alteration pH immediately sampling leads only one reaction product, which stable storable solution at 4°C 2 days.
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