Preparation and tandem mass spectrometric analyses of deuterium-labeled cysteine-containing leukotrienes.
Preparation and tandem mass spectrometric analyses of deuterium-labeled cysteine-containing leukotrienes.
复制标题
氘标记的含半胱氨酸的白三烯的制备和串联质谱分析。
DOI：
10.1002/bms.1200190804
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发表时间：
1990
期刊：
影响因子：
--
通讯作者：
Gaskell,SJ
中科院分区：
文献类型：
--
作者：
Raftery,MJ;Thorne,GC;Orkiszewski,RS;Gaskell,SJ
合成了白三烯（LT） C4， E4和n -乙酰基- E4及其各自的单甲基酯和14,15 - 2h2类似物。用双扇形/四极杆混合质谱仪研究了快速原子轰击（FAB）形成的[M + H]+和[M‐H]−离子的碰撞活化分解。获得了每种分析物的结构信息产物离子谱；所提出的断裂路径与标记和衍生物种的平行数据一致。[M + H]+离子的断裂主要发生在含半胱氨酸（主要是LTC4）或脂质衍生（主要是LTE4）部分的硫醚键断裂，电荷保留。由ltc4和LTE4衍生的[M‐H]−离子的碎片之间观察到更明显的差异；然而，对电荷保留的偏好，与[M + H]+离子破碎所观察到的相似。连续流动FAB质谱法分析正品ltc4时所选择的离子监测显示出低图检出限。
Leukotrienes (LT) C4, E4andN‐acetyl‐E4, their respective monomethyl esters and 14,15‐2H2analogs have been synthesized. The collisionally activated decompositions of the [ M + H]+and [ M ‐ H]−ions formed by fast atom bombardment (FAB) have been studied by tandem mass spectrometry using a hybrid sector/quadrupole instrument. Structurally informative product ion spectra were obtained for each analyte; the fragmentation pathways proposed are consistent with the parallel data obtained for labeled and derivatized species. Fragmentation of [ M + H]+ions occurs prominently via cleavage of the thioether linkage with charge retention on the cysteine‐containing (predominant for LTC4) or lipid‐derived (predominant for LTE4) moieties. More pronounced differences were observed between the fragmentations of [ M ‐ H]−ions derived from LTC4and LTE4; the preference for charge retention, however, parallels that observed for the fragmentation of [ M + H]+ions. Selected ion monitoring during continuous‐flow FAB mass spectrometric analysis of authentic LTC4indicated a low‐picogram detection limit.