Rueppel M L, Suba L A, Marvel J T
Biomed Mass Spectrom. 1976 Feb;3(1):28-31. doi: 10.1002/bms.1200030106.
A general derivatization method has been developed for both primary and secondary aminoalkyl-phosphonic acids. Derivatization is effected by reaction with trifluoroacetic acid and trifluoroacetic acid anhydride followed by esterification using ethereal diazo-n-butane. This method can be used for microgram quantities and permits ready characterization by both gas chromatography and gas chromatography mass spectrometry. The structure of this derivative has been verified by mass spectrometry and proton magnetic resonance. Fragmentation patterns were confirmed by high resolution mass spectrometry, isotope labeling and the formation of derivative analogs.
已开发出一种用于伯氨基和仲氨基烷基膦酸的通用衍生化方法。衍生化通过与三氟乙酸和三氟乙酸酐反应,然后使用乙醚重氮正丁烷进行酯化来实现。该方法可用于微克量,并允许通过气相色谱和气相色谱-质谱轻松表征。该衍生物的结构已通过质谱和质子磁共振得到验证。通过高分辨率质谱、同位素标记和衍生物类似物的形成确定了碎片模式。