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A gas-liquid chromatography-flame ionization detection method is described for measuring plasma levels of eicosatetraynoic acid using eicosatriynoic acid as an internal standard. The technique is simple, rapid, and reproducible. Eicosatetraynoic acid and eicosatriynoic acid behave similarly in the extraction system chosen, yet can be easily resolved by gas-liquid chromatography. Under the conditions of our assay, most plasma fatty acids have a short retention time and are found near the solvent front, whereas, eicosatetraynoic acid and eicosatriynoic acid are retained for 6.9 and 3.75 minutes, respectively.