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

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 mu g L-1. For MDA concentrations of 2.0 and 10.0 mu g L-1 the relative standard deviation was less then 5%. The concentration of MDA in urine was measured to be 0.199 +/- A 0.252 mu mol g(-1) creatinine (0.022 +/- A 0.028 mu mol mmol(-1) creatinine).