Sheeley D M, Reinhold V N
Department of Analytical Chemistry, Glaxo Wellcome Inc., Research Triangle Park, North Carolina 27709, USA.
Anal Chem. 1998 Jul 15;70(14):3053-9. doi: 10.1021/ac9713058.
Several oligosaccharide and N-linked glycan samples have been utilized to evaluate structural detail obtained with an ion trap mass spectrometer (ITMS). Using multistage MS/MS (MSn) in a commercial instrument, linear sequence, linkage, and branching have been studied, as well as the positional isomers within branched glycans. Samples were prepared as methylated derivatives, which amplifies the structurally informative cross-ring and double glycosidic cleavage products associated with interresidue linkage and oligomer branching detail. Spectral analysis of a linear glucose homopolymer demonstrated ITMS to be comparable with data obtained from a triple-quadrupole instrument, and in a study of complex glycans, the feature of MSn enabled the assignment of linkages that cannot be assessed by conventional triple-quadrupole tandem instrumentation. The longer time scale of CID experiments enhances the abundance of multiple bond ruptures important for a complete understanding of structure. This technology appears to provide a significant step toward the goal of characterizing all aspects of carbohydrate structure using a single instrument.
几种寡糖和N-连接聚糖样品已被用于评估离子阱质谱仪（ITMS）所获得的结构细节。使用商用仪器中的多级MS/MS（MSn），研究了线性序列、连接方式和分支情况，以及分支聚糖中的位置异构体。样品制备成甲基化衍生物，这增强了与残基间连接和低聚物分支细节相关的具有结构信息的跨环和双糖苷裂解产物。对线性葡萄糖均聚物的光谱分析表明，ITMS与从三重四极杆仪器获得的数据相当，并且在对复杂聚糖的研究中，MSn的特性使得能够确定常规三重四极杆串联仪器无法评估的连接方式。CID实验较长的时间尺度增加了对完整理解结构至关重要的多键断裂的丰度。这项技术似乎朝着使用单一仪器表征碳水化合物结构所有方面的目标迈出了重要一步。
