Variouss concentrationss of free malonaldehyde were prepared from 1,1,3,3-tetraethoxy propane (TEP). Spectrophoto-metric determination and HPLC analysis of free malonaldehyde instead of malonaldehyde-thiobaribituric acid (MA-TBA) complex were conducted. Malonaldehyde was well separated on a $\mu$Bondapak C18 column. The absorbances at 254 nm and the HPLC peak areas of free malonaldehyde increased with the increase in its concentration. The correlation coefficient between absorbances and peak areas was 0.998. The total time elapsed to conduct the whole procedure was less than 15 minutes. This method directly measured the amount of free malonaldehyde in a short period of time successfully. This procedure is expected to be used as a rapid, accurate and specific means to de-termine the development of lipid oxidation in food.