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Oligosaccharide nuclear magnetic resonance hydrogen spectrum quantitative detection technology

A technology of proton nuclear magnetic resonance spectroscopy and detection technology, which is applied in the fields of analysis by nuclear magnetic resonance, material analysis through resonance, and measurement devices, etc. Testing requirements and other issues

Pending Publication Date: 2022-02-08
五源本草(山东)健康科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Fructo-oligosaccharides are formed by the polymerization of 2-10 identical or different monosaccharides. The sugar chains are polymerized at different positions and lengths, forming different isomers, which leads to the complexity of the composition
In particular, there are isomers with similar structures, which are difficult to further separate and purify. In addition, many active ingredients themselves lack spectrally sensitive molecular structures. Conventional analysis methods cannot meet the requirements of separation and detection of each component, and the detection is very difficult.
More importantly, due to the lack of high-purity standard products of different isomers as reference materials for detection, there has been a lack of uniform and direct detection methods worldwide, resulting in differences between different countries, different companies and even different individuals. The tests done are very different and controversial, which brings many difficulties to the promotion and application of fructooligosaccharides

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  • Oligosaccharide nuclear magnetic resonance hydrogen spectrum quantitative detection technology
  • Oligosaccharide nuclear magnetic resonance hydrogen spectrum quantitative detection technology
  • Oligosaccharide nuclear magnetic resonance hydrogen spectrum quantitative detection technology

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Experimental program
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Effect test

Embodiment 1

[0019] Embodiment 1: A kind of fructo-oligosaccharide NMR quantitative detection method and its verification

[0020] 1.1 Instrument method

[0021] Table Instrument Method Description

[0022]

[0023] 1.2 Analysis method

[0024] Sample preparation: Weigh about 10 mg of fructo-oligosaccharide and about 10 mg of maleic acid, weigh them accurately, put them in the same centrifuge tube, add 1ml of heavy water, dissolve in 20μl of deuterated sodium hydroxide mixed solvent, vortex, and transfer to NMR In the tube, detect according to the above-mentioned instrument method.

[0025] Quantitative method: internal standard method (peak area), select the maleic acid hydrogen peak chemical shift value (6.22-5.82 ppm, 2 hydrogens on the ethylenic bond) (defined as 100%), the peak and fructooligosaccharide NMR There is no interference in the peak of the hydrogen spectrum. Select the integral value at 4.98ppm of fructo-oligosaccharide (2 hydrogens on the sugar end group), and detec...

Embodiment 2

[0088] Embodiment 2: A kind of fructo-oligosaccharide proton nuclear magnetic resonance quantitative detection method

[0089] (1) Determination of fructo-oligosaccharide and internal standard maleic acid in the heavy water of volume ratio 1000:5: the quantitative peak in deuterated sodium hydroxide mixed solvent, the quantitative target peak of fructo-oligosaccharide is chemical shift value 4.98 in fructo-oligosaccharide The hydrogen proton peak in ppm, the quantitative target peak of the internal standard maleic acid is the hydrogen proton peak with a chemical shift value of 6.22-5.82 ppm in the internal standard;

[0090] (2) Set the parameters of the nuclear magnetic resonance spectrometer, including: pulse sequence zg90, detection spectrum width 20ppm, sampling time 3min40s, relaxation delay time 8s, line width factor 0.4Hz, sampling temperature 305K, sampling frequency 16 times;

[0091] (3) Sample preparation: Weigh about 10 mg of fructo-oligosaccharide and about 10 mg ...

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Abstract

The technical scheme discloses an oligosaccharide nuclear magnetic resonance hydrogen spectrum quantitative detection technology for the first time, for a determined nuclear magnetic active atomic nucleus, the nuclear magnetic resonance signal intensity (peak area) is in direct proportion to the number of atoms generating the signal, and by comparing the signal peak area of quantitative protons of a to-be-detected substance with the quantitative signal peak area of a reference substance, the concentration of the to-be-detected substance is determined by an external standard method.

Description

technical field [0001] The invention belongs to the field of measurement and detection of energetic materials, and also belongs to the field of medical technology. It specifically relates to quality detection, in particular to a drug NMR quantitative detection method. Background technique [0002] Oligosaccharides refer to compounds that contain 2-10 glycosidic bonds polymerized. Oligosaccharides are usually small polymers that connect 2-4 monosaccharides through glycosidic bonds. It includes functional oligosaccharides and ordinary oligosaccharides. sugar. [0003] Functional oligosaccharides, also known as non-digestible oligosaccharides, are low-degree polymerized sugars with branched or straight chains formed by dehydration of 2 to 7 monosaccharide molecules connected by α-, β-type and other glycosidic bonds. Certain sweetness, viscosity and water-solubility characteristics of sugars, such as fructo-oligosaccharides, raffinose, isomaltulose and so on. [0004] Fructo-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N24/08G01N1/28
CPCG01N24/082G01N1/28
Inventor 邵成雷路杰李凯李振鹏吴立民胡星吉朱冬芮
Owner 五源本草(山东)健康科技有限公司