期刊名称:Journal of Nutritional Science and Vitaminology
印刷版ISSN:0301-4800
电子版ISSN:1881-7742
出版年度:1980
卷号:26
期号:1
页码:77-85
DOI:10.3177/jnsv.26.77
出版社:Center for Academic Publications Japan
摘要:L-[2', 3', 5', 6'-d]Tyrosine (Tyr-d4) and L-[2', 6'-d]Tyr (Tyr-d2) were prepared. Tyr was heated in conc. DCl at 180°C for 4 hr to obtain DL-[2, 2', 3', 5', 6'-d]Tyr '(Tyr-d5), then the deuterium on the 2-position of the compound was successfully replaced with proton by refluxing with an acetic acid-acetic anhydride mixture. The isotopic purity of DL-Tyr-d4 was about 60%. The racemic mixture was resolved enzymatically. L-Tyr-d2 was prepared by refluxing the resultant Tyr-d4 with 5.5 N HCI. The deuterated amino acids were analyzed as the N, O -bis (trifluoroacetyl) methyl ester or N, O -bis(heptafluorobutyryl) methyl ester derivatives by the gas chromatography-selective ion monitoring method (SIM). The calibration curves showed good linearity in the range where the molar ratios of Tyr-d4/Tyr-do and Tyr-d2/Tyr-do were above 5/1, 000. The results indicate that the protein-bound Tyr-d4 may possibly be determined as Tyr-d2 after hydrolysis of protein.
关键词:tyrosine;gas chromatography-mass spectrometry;selective ion monitoring;deuterium;labeling