APPLICATION OF CRYOGENIC NMR PROBES

Abstract

Abstract:

In the past decade manufactures of NMR systems have put many efforts into the re search and development of new NMR probe technologies. Recently the development o f cryogenically cooled NMR probe has been the subject of considerable interest i n the light of the large sensitivity gains they may provide, and hence the savin gs in acquisition time by using this technology. For low gamma nuclides, such as ¹⁵N, the advantages that cryogenic NMR probes provide in terms of det ection sen sitivity and acquisition time may, in a sense more important than the enhancemen t of sensitivity per se, provide the opportunity of direct detection of NMR sign als in their natural abundances, while isotopeenriched samples often have to b e used when conventional NMR probes are employed. In this study, 5～10 Hz optimi ze d CIGAR-HMBC ¹H-¹⁵N experiments were performed on a 2 mg natural a bundance sampl e of the oxazolidinone antibiotic eperezolid in a 3 mm NMR tube using a 5 mm Varian ¹H-¹⁵N Cryo-QNMR probe and a 3 mm gradient inverse triple res onance probe, and the results from the two probes were compared. With the cryogenic NMR probe, a ¹H-¹⁵N CIGAR-HMBC spectrum, in which most previously reportedlong -range coup lings were observed, was recorded in ～10 min. Almost all of the expected long-r ange responses were observed when the acquisition time was increased to 26 min. The same experiment using the conventional probe gave data that were of substant ially lower quality. About four hours were required for the conventional probe t o acquire a spectrum that displayed all the coupling responses as those shown by the 26 min cryogenic probe spectrum. Eighteen hours of acquisition time were re quired for the conventional probe to obtain a spectrum that was comparable in terms of signal-to-noise ratio to that obtained by the cryogenic probe in 26 min.

Key words: NMR, cryogenic NMR probe, HMBC, long-range 1H-15N NMR, natural abundance

CLC Number:

O482.53

FENG Rui, XIE Hua, REN Da-zhou. APPLICATION OF CRYOGENIC NMR PROBES[J]. Chinese Journal of Magnetic Resonance.

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