The causes responsible for the low reproducibility of the gas chromato
graphic method used to analyze fatty acid methyl esters, derived from
the transesterification of triglycerides in n-hexane by means of metha
nol potassium hydroxide, were identified and eliminated. Partition coe
fficients (Kd) of short-chain fatty acid methyl esters between n-hexan
e and methanol were determined. These results indicate that even under
the best experimental conditions, a substantial portion of these comp
ounds are transferred in the methanol phase and therefore are not anal
yzed. Accurate results, to within 2% were obtained by rigorously contr
olling the volume of the reagents and introducing appropriate correcti
on factors. The accuracy of the results, reported as a percentage by w
eight, did not depend on the completeness of the transesterification r
eaction. In the analysis of fatty acids as butyl eaters, a measurable
quantity of butyric ester was lost during the washing phase with water
. By contract, butyric acid pentyl ester is insoluble in water. Theref
ore we propose an accurate method to analyze fatty acids as pentyl est
ers. Oleic and elaidinic acids derived from triglyceride transesterifi
cation are easier to separate as methyl esters than as longer butyl or
pentyl esters.