Lee T A, Frost D I, Wilson G E, Hardy J K
Department of Chemistry, University of Akron, Ohio 44325.
Anal Biochem. 1991 Sep 2;197(2):321-5. doi: 10.1016/0003-2697(91)90399-e.
A method for determining the position and enrichment of isotope labels in amino acids using gas chromatography/mass spectrometry is described. [alpha-15N]- and [epsilon-15N]lysine, [1-13C]- and [15N]alanine and -leucine, and [1-13C]-, [2-13C]-, [3-13C]-, and [4-13C]aspartic acid were investigated. Standards for each isotope label were prepared and analyzed under scan conditions, and line pairs characteristic for the label were identified. The standards were reanalyzed under selective ion monitoring conditions to verify the behavior of the line pairs. Mixtures of amino acids containing different isotope labels or the same label in different positions were prepared and analyzed under selective ion monitoring conditions. Enrichments were determined with high precision and relative errors ranging from 0.14 to 36%.
描述了一种使用气相色谱/质谱法测定氨基酸中同位素标记的位置和富集情况的方法。研究了[α-¹⁵N]-和[ε-¹⁵N]赖氨酸、[¹-¹³C]-和[¹⁵N]丙氨酸及亮氨酸,以及[¹-¹³C]-、[²-¹³C]-、[³-¹³C]-和[⁴-¹³C]天冬氨酸。制备了每种同位素标记的标准品,并在扫描条件下进行分析,识别出该标记的特征线对。在选择性离子监测条件下对标准品进行重新分析,以验证线对的行为。制备了含有不同同位素标记或同一标记处于不同位置的氨基酸混合物,并在选择性离子监测条件下进行分析。富集情况测定精度高,相对误差范围为0.14%至36%。