Procedures for structural analysis of fatty acids are reviewed. The em
phasis is on methods that involve gas chromatography-mass spectrometry
and, in particular, the use of picolinyl ester and dimethyloxazoline
derivatives. These should be considered as complementing each other, n
ot simply as alternatives. However, additional derivatization procedur
es can be of value, including hydrogenation and deuteration, and prepa
ration of dimethyl disulfide and 4-methyl-1,2,4-triazoline-3,5-dione a
dducts. Sometimes complex mixtures must be separated into simpler frac
tions prior to analysis by gas chromatography-mass spectrometry. Silve
r ion and reversed-phase highperformance liquid chromatography are the
n of special value. In particular, a novel application of the latter t
echnique, involving a base-deactivated stationary phase and acetonitri
le as mobile phase, is described that is suited to the separation of f
atty acids in the form of picolinyl ester and dimethyloxazoline deriva
tives, as well as methyl esters.