Various concentrations of malonaldehyde (MA) produced upon hydrolysis of 1, 1, 3,3-tetraethoxypropane (TEP) were reacted with 2-thiobarbituric acid (TBA)and th e contents of MA-TBA complex were measured both with spectrophotometer and high performance liquid chromatography (HPLC). As the concentrations of MA-TBA increased, their absorbances and the corresponding HPLC peak areas increased. The correlation coefficient between absorbances and HPLC peak areas of MA-TBA peaks from the other compounds and butanol extraction of the complex increased its recovery its recovery by 29.4% . Measurement of the content of MA-TBA complex for monitoring the development of lipid oxidation was proven to be successful with the use of high performance liquid chromatography.