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通过核磁共振光谱法利用质子间接检测固体中的氮-14。

Indirect detection of nitrogen-14 in solids via protons by nuclear magnetic resonance spectroscopy.

作者信息

Cavadini Simone, Antonijevic Sasa, Lupulescu Adonis, Bodenhausen Geoffrey

机构信息

Laboratoire de Résonance Magnétique Biomoléculaire, Institut des Sciences et Ingénierie Chimiques, Ecole Polytechnique Fédérale de Lausanne, Batochime, CH-1015 Lausanne, Switzerland.

出版信息

J Magn Reson. 2006 Sep;182(1):168-72. doi: 10.1016/j.jmr.2006.06.003. Epub 2006 Jun 27.

Abstract

This Communication describes the indirect detection of 14N nuclei (spin I=1) in solids by nuclear magnetic resonance (NMR) spectroscopy. The two-dimensional correlation method used here is closely related to the heteronuclear multiple quantum correlation (HMQC) experiment introduced in 1979 to study molecules in liquids, which has recently been used to study solids spinning at the magic angle. The difference is that the coherence transfer from neighboring 1H nuclei to 14N is achieved via a combination of J couplings and residual dipolar splittings (RDS). Projections of the two-dimensional correlation spectra onto the 14N dimension yield powder patterns which reflect the 14N quadrupolar interaction. In contrast to the indirect detection of 14N via 13C nuclei that was recently demonstrated [Gan, J. Am. Chem. Soc. 128 (2006) 6040; Cavadini et. al., J. Am. Chem. Soc., 128 (2006) 7706], this approach may benefit from enhanced sensitivity, and does not require isotopic enrichment in 13C, although the 1H line-widths may have to be reduced upon selective deuteration.

摘要

本通讯描述了通过核磁共振(NMR)光谱法间接检测固体中的14N原子核(自旋I = 1)。这里使用的二维相关方法与1979年引入的用于研究液体中分子的异核多量子相关(HMQC)实验密切相关,该实验最近已被用于研究以魔角旋转的固体。不同之处在于,相邻1H原子核到14N的相干转移是通过J耦合和残余偶极分裂(RDS)的组合实现的。二维相关光谱在14N维度上的投影产生反映14N四极相互作用的粉末图谱。与最近证明的通过13C原子核间接检测14N的方法[Gan,J. Am. Chem. Soc. 128 (2006) 6040;Cavadini等人,J. Am. Chem. Soc.,128 (2006) 7706]相比,这种方法可能受益于更高的灵敏度,并且不需要13C同位素富集,尽管在选择性氘代时可能必须减小1H线宽。

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