Dünnschicht- und Gaschromatographie von Tocopherolen

Thin-Layer end Gas Chromatography of Tocopherols Oilseeds, to which an internal standard of tocopherol was given, were extracted for tocopherols with ethanol under conditions inhibiting oxidation using an Ultra-Turrax homogenizer. After filtration the ethanolic extract is briefly saponified and the unsaponifiable matter containing the tocopherols extracted into n-hexane. Then the hexane-fraction is washed alkalifree with water, dried over Na₂SO₄, concentrated and applied on a silicagel GF₂₅₄-plate, which is developed with dichloromethane. With co-chromatographed reference-tocopherols on the margins of the TLC-plate the presence of tocopherolquinones can be checked in UV-light, whereas the bands of tocopherols and tocotrienols are located by spraying the margins with Emmerie and Engel-reagent. The corresponding zones were scrapped off the plate, the silicagel extracted with 15 × 1 ml ethanol, the ethanol evaporated to dryness and the residue derivatised to trimethylsilylethers. Gaschromatography on 3 m SE-52/XE-60 or 1.5 m SE-30 columns gave a good separation of tocopherols and tocotrienols. Simultaneous qualitative and quantitative determination of tocopherols by GLC combined with the possibility of automation makes this analytical procedure superior to TLC and colorimetry of tocopherols. About 500 tests with different oilseeds in the range between 50-800 mg lipid and 20-2000 μg of total tocopherol/sample gave a recovery of 60% at a coefficient of variation of approximately 6%.