AbstractThe separation of the toxicologically important aldehyde acrolein from other carbonyl compounds by high performance liquid chromatography after derivatization to 2,4‐dinitrophenylhydrazones is critically discussed on the basis of a selection of published methods. A method is proposed whereby the compounds acrolein, acetone, and propanal may be reproducibly separated to baseline by a reversed phase HPLC procedure employing a ternary mixture of methanol, water, and acetonitrile as mobile phas