High-sensitive three-dimensional nuclear magnetic resonance spectrum method

Abstract

The invention provides a high-sensitive three-dimensional nuclear magnetic resonance spectrum method. The method comprises the following steps: applying proton 90-DEG hard pulse, performing delay, andthen simultaneously applying proton and X-nuclear 180-DEG hard pulse, and then performing delay; and then simultaneously performing proton and X-nuclear 90-DEG hard pulse, performing delay, applyingproton 180-DEG hard pulse, and then performing delay, applying SMSQ10.100 gradient field pulse; applying X-nuclear 180-DEG hard pulse, and then performing delaying, simultaneously applying proton andX-nuclear 90-DEG hard pulse, and performing delay, applying proton 180-DEG hard pulse; and then performing delay, applying X-nuclear 180-DEG hard pulse; performing delay, applying TOCSY self-spinninglocking combined pulse, and then performing delay for theta, applying proton 180-DEG hard pulse, and then applying SMSQ 10.100 gradient field pulse, beginning sampling, wherein the Garp combined pulsedecoupling is performed on the X-nuclear at the sampling period. The three-dimensional Fourier transform is performed on the data, thereby obtaining the HSQC-TQCSY magnetic nuclear resonance spectrum.

Description

technical field [0001] The invention relates to a nuclear magnetic resonance spectroscopy detection method, in particular to a highly sensitive three-dimensional nuclear magnetic resonance spectroscopy method. Background technique [0002] Determination of the composition of complex architectures such as biological polysaccharides, biological oligosaccharides, mineral-derived oils and synthetic oils has always been an important part of the research on glycobiology and oil refining. The most traditional analytical methods in the detection of biological polysaccharides, oligosaccharides and oils are mass spectrometry (MS) and nuclear magnetic resonance (NMR). Although mass spectrometry has obvious advantages in detection sensitivity, it has obvious disadvantages in the detection of biological polysaccharides and oligosaccharides with branched chain structures and oil products. On the contrary, although nuclear magnetic resonance technology has obvious advantages in the struct...

AI Technical Summary

Problems solved by technology

For conventional NMR, even the two-dimensional spectrum of oil products is affected by serious signal overlap; although three-dimensional NMR spectrum can solve the problem of serious signal overlap in two-dimensional spectrum, the sensitivity of conventional three-dimensional spectrum will be seriously affected, making the experiment The time is too long to become unrealistic, which limits the application of 3D NMR spectroscopy in the field of oil analysis

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