Analysis of amino acids by gas-liquid chromatography as tert.-butyldimethylsilyl derivatives. Preparation of derivatives in a single reaction.
The effect of temperature, solvent and reagents on the formation of the N(O)-dimethyl-tert.-butylsilyl derivatives of proteic amino acids has been studied. Quantitative silylation is achieved using dimethyl-tert.-butylsilyltrifluoroacetamide with 1% tert.-butyldimethylchlorosilane in dimethylformamide by heating at 75 degrees C for 30 min. Two peaks were obtained for arginine under these conditions. However, most of the standard proteic amino acids can be assayed. The N(O)-dimethyl-tert.-butylsilyl derivatives of the proteic amino acids have been analysed by gas chromatography-mass spectrometry using the methane chemical ionization mode. The spectral data are presented and have been used to confirm the structures of the amino acid derivatives.
D000596:Amino Acids / Q000032:analysis*; D001120:Arginine / Q000032:analysis; D002384:Catalysis; D055598:Chemical Phenomena; D002621:Chemistry; D002849:Chromatography, Gas; D004355:Drug Stability; D007202:Indicators and Reagents; D013058:Mass Spectrometry; D017646:Organosilicon Compounds; D012825:Silicon / Q000032:analysis*; D012997:Solvents; D013696:Temperature
D000596:Amino Acids; D007202:Indicators and Reagents; D017646:Organosilicon Compounds; D012997:Solvents; C009660:t-butyldimethylsilyl compounds; D001120:Arginine; D012825:Silicon