Recebido em 16/2/07; aceito em 7/3/08; publicado na web em 31/10/08Free radicals induce lipid peroxidation, playing an important role in patho logical processes. The injury mediated by free radicals can be measured by conjugated dienes, malon dial dehyde, 4-hydroxynonenal, and others. However, malondialdehyde has been pointed out as the main product to evaluate lipid peroxidation. Most assays determine malondialdehyde by its reaction with thiobarbituric acid, which can be mea sured by indirect (spectrometry) and direct methodologies (chromatography). Though there is some controversy among the methodologies, the selective HPLC-based assays provide a more reliable lipid peroxidation measure. This review describes significant aspects about MDA deter mination, its importance in pathologies and biological samples treatment.