抄録
Trifluoroacetyl (TFA) derivatives of sugars has many merits in simplicity and rapidness of preparation, volatility on non selective columns and excellent separation of alditols.
We examined trifluoroacetylation by trifluoroacetic anhydride (TFAA) in tetrahydrofuran (THF), acetonitrile and ethyl acetate (AcEt) and effects of the solvents on the formation of the TFA derivatives.
The recommended procedure of trifluoroacetylation was established as follows: To 100-500 μg of sugars, 0.3 ml of THF (or AcEt) and 0.1 ml of TFAA was added. The mixture was kept for 10 min at 40°C. 1-2, μl of the solution was injected into a gas chromatograph.
All gas chromatographic analysis were conducted on a Shimadzu GC-1C gas chromatograph equipped with a hydrogen flame ionization detector. Glass tubes (150 cm in length and 4 mm i. d.) were packed with various liquid phases coated on Gas-Chrom P (80-100 mesh). Nitrogen was used as the carrier gas at a flow rate of 90 ml/min.
To prevent multiplicity of peaks, reduction of sugars to their alditols and separation of 11 alditols was performed on 2% CNSi column as TFA derivatives. Then, we studied hydrolysis of oligosaccharides in glycoprotein by trifluoroacetic acid. The established method of hydrolysis made it possible to apply gas chromatography to analysis of neutral sugars combined with serum protein.
