This chapter has outlined methods to assess lipid peroxidation associated with oxidant injury in vivo by quantifying concentrations of free F2-IsoPs in biological fluids and levels of F2-IsoPs esterified in tissue lipids. The mass spectrometric assay described herein is highly precise and accurate. A potential shortcoming with this approach is that it requires expensive instrumentation, i.e., a mass spectrometer. However, several immunoassays for an F2-IsoP, 8-iso-PGF2 alpha, have become available from commercial sources. At this time, the accuracy and reliability of these assay for quantifying F2-IsoPs in biological fluids has not been fully validated by mass spectrometry. If these immunoassays prove to be a reliable measure of F2-IsoPs, however, this should greatly expand the use of F2-IsoPs to assess oxidant stress. In conclusion, studies carried out over the past several years have shown that measurement of F2-IsoPs has overcome many of the limitations associated with other methods to assess oxidant status, especially when applied to the measurement of oxidant stress in vivo in humans. Therefore, the quantification of F2-IsoPs represents an important advance in our ability to assess the role of oxidant stress and lipid peroxidation in human disease.