Determination of tocopherols and sterols by capillary gas chromatography

Abstract A method is described for simultaneously determining tocopherols and sterols in fats and oils by quantitative capillary gas chromatography. Samples containing ca. 100 mg of lipid were saponified in capped tubes with aqueous KOH by heating for 8 min at 80 C; the unsaponifiable fraction was extracted with cyclohexane, freed of solvent, derivatized to form the trimethylsilyl ethers of both tocopherols and sterols, and chromatographed on a 50 m×0.25 mm glass capillary column coated with Dexsil 400. Most of the individual tocopherols and common sterols were well separated, although interfering peaks were seen in some samples, which for better specificity should be subjected to an initial purification. For most samples, however, the simplified sample preparation, without preliminary purification, was adequate when combined with capillary gas chromatography. Recovery, method and gas liquid chromatographic precision, and applications are discussed.