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• W2037268575 abstract "Recently, a variety of schemes for obtaining 2D heteronuclear RELAY spectra have been proposed (I-6). These methods can be quite powerful for structure determination and spectral assignment. However, a recent analysis (7) has shown that in many cases the sensitivity of heteronuclear relayed-magnetization-transfer spectroscopy is considerably lower than for heteronuclear chemical-shift correlation (8-10). Especially in compounds with saturated aliphatic ring systems, such as steroids and alkaloids, the sensitivity of the heteronuclear RELAY experiment is often very low. Moreover, in all heteronuclear RELAY experiments proposed so far the ‘H-‘H multiplet components of the (‘H-13C) RELAY multiplet are in antiphase relative to one another (analogous to the antiphase nature of multiplet components in a COSY spectrum (II)) and the ‘H-13C RELAY multiplet is 90” out of phase relative to nonrelayed signal in the 2D spectrum. No pure-absorption 2D spectra can therefore be recorded with the existing RELAY experiments. We propose a new pulse scheme for heteronuclear RELAY spectroscopy that partly overcomes the problems mentioned above. In the new scheme, net magnetization transfer among protons is achieved via homonuclear Hartmann-Hahn-type cross-polarization. This type of homonuclear magnetization transfer was first discovered (12) as an artifact in homonuclear transverse NOE spectroscopy (13) and is closely related to the magnetization-transfer mechanism in the TOCSY experiment (14). We have recently demonstrated that this type of homonuclear cross-polarization is very powerful for the assignment of complex proton spectra (15). The possibility of obtaining net magnetization transfer in coupled ‘H spin systems makes this approach very suitable for heteronuclear RELAY spectroscopy. The pulse scheme of the new method is sketched in Fig. 1. An alternating spinlock field along the fx axis of the proton rotating frame provides the crucial mechanism for homonuclear Hartmann-Hahn-type cross-polarization. Consider first, for reasons of simplicity, a rf field of nominal strength, v = yH2/27r, that is continuously aligned along the x axis of the proton. rotating frame. Two protons, A and B, with offset frequencies AA and AB, experience effective rf field strengths, VA and VB . Provided that v s AA, AB, VA and VB are to a good approximation given by" @default.
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• W2037268575 date "1985-06-01" @default.
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• W2037268575 title "An improved method for two-dimensional heteronuclear relayed-coherence-transfer NMR spectroscopy" @default.
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• W2037268575 doi "https://doi.org/10.1016/0022-2364(85)90176-3" @default.
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