Derivatization reagents and procedures were studied for the preparation of trifluoroacetyl derivatives of carbohydrates. It was found that N-methylbis(trifluoroacetamide), MBTFA, produced the corresponding trifluoroacetates of the mono-, di-, tri-, and tetrasaccharides studied. When subjected to gas chromatography, quantitative results were obtained with the derivatives yielding a high degree of volatility. The high volatility gave single-run analysis capabilities for sugar mixtures containing mono- through tetrasaccharides in as little as 15 minutes with chromatographic conditions less severe than previously required for other methods.