Betulin (1) is a naturally occurring pentacyclic triterpene that can be isolated up to 28% from the dry mass of birch bark. The extraction process provides technical product which besides betulin (~70% assay) contains also betulinic acid, lupeol, etc. [2]. This project is devoted for research of superior analytical procedures for derivatization purposes of such natural compounds for gas chromatography using Vogel’s silyl sulfinates 3a and 3b [2]. The latter were compared to other commercially available reagents used for silylation [3].