Lipids are important molecules, serving as feedstocks in chemical industry as well as providing vital functions within all living organisms. They figure prominently in the development and production of many commodities, including biofuels. Analysis of these molecules is essential in both medicinal and industrial fields. In this paper, acid-catalyzed transesterification reactions were performed on coconut oil, red palm oil, and safflower oil to to establish a simple, effective method for analysis that can be applied to algal lipid analysis. Parameters for analysis of the resulting fatty acid methyl esters (FAME) by gas chromatography mass spectrometry (GC-MS) were honed and optimized, and a reliable, efficient procedure was developed.