Determination of malondialdehyde in human blood by headspace-solid phase micro-extraction gas chromatography-mass spectrometry after derivatization with 2,2,2-trifluoroethylhydrazine.
Malondialdehyde (MDA) has been proposed as a useful biomarker of lipoperoxidation in biological samples, and more developed analytical methods are necessary. A simple and sensitive gas chromatography-mass spectrometry (HS-SPME-GC-MS) was described for the determination of malondialdehyde (MDA) in blood. Acetone-d(6) was used as internal standard. MDA and acetone d6 in blood reacted for 40 min at 50 degrees C with 2,2,2-trifluoroethylhydrazine in headspace vial and simultaneously the formed TFEH derivatives were vaporized and adsorbed on polydimethylsiloxane-divinylbenzene (PDMS-DVB). The compounds were desorbed for 1 min at 240 degrees C and injected in GC-MS. The reaction solution showed good recoveries at pH 4.0. In the established condition, the method detection limit (MDL) was 0.4 microg/L in 0.1 mL blood sample and the relative standard deviation was less than 8% at the concentration of 25.0 and 50.0 microg/L. The mean concentrations of MDA in normal human blood (n=20) were measured to be 187.9 microg/L (2.61 micromol/L).
Shin
Ho-Sang
HS
Department of Environmental Education, Kongju National University, Kongju 314-701, Republic of Korea. hshin@kongju.ac.kr
D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D006834:Hydrazines / Q000737:chemistry*; D008315:Malondialdehyde / Q000097:blood* / Q000737:chemistry*; D052617:Solid Phase Microextraction / Q000379:methods*
D006834:Hydrazines; C007675:ethylhydrazine; D008315:Malondialdehyde