Sensitive Analysis of Malondialdehyde in Human Urine by Derivatization with Pentafluorophenylhydrazine then Headspace GC–MS

Abstract

A sensitive method based on derivatization with pentafluorophenylhydrazine then headspace gas chromatography–mass spectrometry has been used for analysis of malondialdehyde in human urine. Preparation of urine sample by one-step derivatization/evaporation was performed by reaction of malondialdehyde with pentafluorophenylhydrazine in a headspace vial for 10 min; the derivatives were then injected in GC–MS analysis. The reaction was performed at pH 3, and total analysis time was 35 min. The method detection limit was 0.04 μg L−1. For MDA concentrations of 2.0 and 10.0 μg L−1 the relative standard deviation was less then 5%. The concentration of MDA in urine was measured to be 0.199 ± 0.252 μmol g−1 creatinine (0.022 ± 0.028 μmol mmol−1 creatinine).