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首页> 外文期刊>Journal of magnetic resonance >Selective heteronuclear Hartmann–Hahn: A multiple-pulse sequence for selective magnetization transfer in the structural elucidation of ‘‘isotagged” oligosaccharides
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Selective heteronuclear Hartmann–Hahn: A multiple-pulse sequence for selective magnetization transfer in the structural elucidation of ‘‘isotagged” oligosaccharides

机译：选择性异核Hartmann-Hahn：在“ isotagged”寡糖的结构解析中用于选择性磁化转移的多脉冲序列

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摘要

A new selective heteronuclear Hartmann–Hahn (SHEHAHA) multiple-pulse mixing sequence is proposed for the solution structure elucidation of milligram amounts of peracetylated oligosaccharides in which the acetyl groups are enriched in carbon-13, so-called ‘‘isotags”. SHEHAHA accomplishes exclusive inphase magnetization transfer between the isotag carbonyl 13C and the proximal proton on the sugar ring. Relayed transfer around the sugar rings by proton–proton TOCSY is suppressed, while the heteronuclear transfer from the labeled carbonyl carbon to the proximal ring proton is maintained. The sequence is broadband in the sense that all acetyl groups simultaneously give good signal transfer to their respective nearest proton neighbors. The 1H-detected spectra have decent sensitivity and excellent resolution, giving patterns that unambiguously identify common structural subunits in human glycans. Peracetylated maltitol is shown as a test case of the method. Lineshapes are pure absorption, allowing facile measurement of vicinal proton–proton couplings. Linkage points can be deduced, and the 2D correlation spectra may be useful for more ambitious prediction algorithms and machine identification by a spectral database.
机译：提出了一种新的选择性异核Hartmann-Hahn（SHEHAHA）多脉冲混合序列，用于阐明毫克量的过乙酰化寡糖的溶液结构，其中乙酰基富含13碳，即所谓的“ isotags”。 SHEHAHA完成了isotag羰基13C和糖环上近端质子之间的独家同相磁化转移。质子-质子TOCSY抑制了糖环周围的接力转移，同时保持了从标记的羰基碳到近端环质子的异核转移。从所有乙酰基同时向其各自最近的质子邻域传递良好信号的意义上讲，该序列是宽带的。检测到的1H光谱具有不错的灵敏度和出色的分离度，所给出的图谱可以明确识别人聚糖中的常见结构亚基。显示了过乙酰化的麦芽糖醇作为该方法的测试案例。线形是纯吸收性的，可以轻松测量附近的质子-质子耦合。可以推断出链接点，并且2D相关光谱对于光谱数据库更雄心勃勃的预测算法和机器识别很有用。

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