A method for the determination of fatty acid methyl esters in biodiesel was investigated by gas chromatography using a stainless steel column packed with polydiethylene glycol adipate coated on 102 white support and a flame ionization detector. The linear correlation coefficient was above 0.998, the relative standard deviation was less than 0.46%, and the recovery of standard addition was found to be within 96.8–105.4%. It has good separation efficiency, accuracy, and reproducibility.