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Measurement method of isomaltulose heteronuclear long-range coupling spectrum based on nuclear magnetic resonance technology
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A technology of isomaltulose and nuclear magnetic resonance, which is applied in the field of chemical analysis and can solve problems such as slow speed
Active Publication Date: 2022-08-02
ZHEJIANG UNIV
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Similar to sucrose, it is composed of glucose and fructose molecules, but the linkages between the molecules are stronger than sucrose, which means it is fully digested by the body, but more slowly
However, there is no report on the test method of isomaltulose heteronuclear long-range coupling spectrum (Constant time inverse-detection gradient accordion rescaled long-range correlation, CIGAR)
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Embodiment 1
[0037] The specific steps of isomaltulose CIGAR spectrum determination are as follows:
[0038] Step 1, weigh isomaltulose and put it into a test tube, add deuterated dimethyl sulfoxide, the ratio of the mass to volume of isomaltulose and deuterated dimethyl sulfoxide is 30mg: 0.6mL, ultrasonically dissolve fully, transfer into NMR tube, and then put the test tube filled with the sample into the detection magnet of the NMR spectrometer;
[0039] Step 2, select the corresponding deuterated solvent in the instrument workstation, and perform tuning, shimming and field locking;
[0040] Step 3, Setup 1 Test parameters of H: Turn on the pulse sequence, and set the experimental conditions including the direct dimension spectral width, the number of scans, and the acquisition mode; this is the preparation for step 6.
[0041] Among them, the main content of the pulse sequence is: taking hydrogen as the observation nucleus, after a relaxation delay time (d1), the magnetization vecto...
Embodiment 2
[0051] As shown in Table 1, different single bond coupling constants are optimized on the basis of Example 1, and the maximum and minimum values of the single bond coupling constants are set as (5,3), (8,5), (10,6), it is found that when the maximum value is 8Hz and the minimum value is 5Hz, the number of CIGAR correlation points measured is the largest and basically stable, so the maximum value is 8Hz and the minimum value is 5Hz.
[0052] Table 1. Signal correspondence table of CIGAR spectra of samples under different single-bond coupling constant settings
[0053]
Embodiment 3
[0055] As shown in Table 2, in this embodiment, the detected direct dimension spectral width (sw) is 9615 Hz. On the basis of Embodiment 1, the single sampling time (at) of the sampling period is adjusted, and is set from 150ms to 100ms and 200ms. It is found that the number of measured ROE correlation points varies greatly, indicating that the optimization of the sampling time is more effective, so the preferred sampling time at is 149.968ms.
[0056] Table 2. Signal correspondence table of CIGAR spectra of samples at different sampling times (at)
[0057] serial number Sampling time (ms) Number of CIGAR correlation points 1 at=100.035 12 2 at=149.968 15 3 at=199.547 13
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Abstract
The invention discloses a method for testing isomaltulose heteronuclear long-range coupling spectrum based on nuclear magnetic resonance technology, and belongs to the technical field of chemical analysis. The steps of the method include: (1) dissolving isomaltulose in deuterated dimethyl sulfoxide, transferring it to a nuclear magnetic tube, and placing the nuclear magnetic tube into a detection magnet of a nuclear magnetic spectrometer; (2) in a workstation Select the solvent deuterated dimethyl sulfoxide, perform tuning, shimming and field locking; (3) Load the pulse sequence optimization and set other detection parameters; (4) After completing the settings, execute the program to obtain the heteronuclear long-range of isomaltulose coupled spectrum. The method adopts three-step low-pass filter and adiabatic conditions, and optimizes the pulse sequence to measure the isomaltulose heteronuclear long-range coupling spectrum, which provides a simple and effective method for the heteronuclear long-range coupling conformation determination of isomaltulose samples. s method.
Description
technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a method for testing isomaltulose heteronuclear long-range coupled spectroscopy (CIGAR) based on nuclear magnetic resonance technology. Background technique [0002] Isomaltulose, derived from sugar beet, is a natural sugar with a unique molecular structure. Similar to sucrose, it is composed of glucose and fructose molecules, but its intermolecular linkages are stronger than sucrose, which means it can be fully digested by the body, but more slowly. As a natural ingredient that releases carbohydrates slowly, isomaltulose provides complete carbohydrate energy (glucose) in a more stable and sustained manner, while maintaining blood sugar balance, allowing the body to utilize carbohydrates over a longer period of time Compound energy source. At the same time, it is widely used in various foods and sweeteners because of its excellent taste, low sweetness and tooth decay-...
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