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Method for determining branching degree of glucose polymer by using nuclear magnetic resonance

A glucose polymer and nuclear magnetic resonance technology, applied in the direction of nuclear magnetic resonance analysis, etc., can solve the problems of difficult operation, inability to measure the degree of branching, poor reproducibility, etc., and achieve the effect of improving the measurement accuracy and simplifying the measurement steps

Inactive Publication Date: 2018-05-11
青岛力腾医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The structural analysis of starch by traditional chemical methods, especially the determination of the starch connection method, is cumbersome and difficult to operate. There are large differences in the determination of structures between different methods, and the reproducibility is poor.
[0004] Among the spectroscopic methods, ultraviolet spectrophotometry mainly determines the ratio of amylose, amylopectin and iodine by the difference in the maximum absorption wavelength of the compound, which is not suitable for glucose polymers with relatively small molecular weights; infrared spectroscopy is mainly used for the analysis of starch Identification of groups, cannot be used for determination of degree of branching

Method used

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  • Method for determining branching degree of glucose polymer by using nuclear magnetic resonance
  • Method for determining branching degree of glucose polymer by using nuclear magnetic resonance
  • Method for determining branching degree of glucose polymer by using nuclear magnetic resonance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Weigh 20 mg of icodextrin and place it in a 5 mm sample test tube, add about 0.6 ml of heavy water to dissolve, make the prepared solution reach a depth of 3-4 cm in the sample test tube, cover the NMR cap, and follow the one-dimensional hydrogen Spectrum or carbon spectrum operation requires operation, NMR analysis results such as figure 1 As shown, the following table is made according to the conclusions that can be drawn from the figure:

[0034] Assignment of each peak: 5.2ppm

[0035]

[0036] Through the above results, the degree of branching is calculated:

[0037] Sample branching degree=0.37 / (7.51+1.11+0.37)*100%=4.12%

Embodiment 2

[0039] Take 20 mg of icodextrin and place it in a 5mm sample test tube, add about 0.6ml of heavy water to dissolve it, make the prepared solution reach a depth of 3-4 cm in the sample test tube, cover the NMR cap, and analyze according to the one-dimensional hydrogen spectrum The operation requires operation, suppresses the water peak, and the nuclear magnetic resonance analysis results are as follows figure 2 shown, and according to figure 2 The conclusions drawn in are tabulated below:

[0040] Assignment of each peak: 5.3ppm

[0041]

[0042] Through the above results, the degree of branching is calculated:

[0043] Sample branching degree=2.23 / (18.82+6.75+2.23)=8.02%

Embodiment 3

[0045] Weigh 20 mg of icodextrin and place it in a 5 mm sample test tube, add about 0.6 ml of heavy water to dissolve, make the prepared solution reach a depth of 3-4 cm in the sample test tube, cover the NMR cap, and follow the one-dimensional carbon The operation of the spectrum requires operation, and the results of the NMR analysis are as follows: image 3 and Figure 4 shown, and make the following table according to the conclusions drawn in the figure:

[0046] The peaks belong to:

[0047] chemical shift ppm

99.85

76.23-78.06

72.79-73.40

71.28-71.83

70.47

69.44

60.56

C positioning

C1

C4

C2

C3, C5

C4

C6

C6

Integral area

1.028

1.013

1.288

2.025

0.186

0.109

1.00

[0048] Through the above results, the degree of branching is calculated:

[0049] Sample branching degree=0.109 / (0.109+1.0)*100%=9.83%

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Abstract

The invention relates to a method for determining the branching degree of a glucose polymer, and especially relates to a method for determining the branching degree of the glucose polymer by using nuclear magnetic resonance. The method concretely includes the following steps: dissolving the glucose polymer to be tested in a solvent to form a solution, determining the hydrogen spectrum or carbon spectrum signal integral intensity of the obtained solution by using a nuclear magnetic resonance spectrometer, and analyzing and calculating the branching degree according to the hydrogen spectrum or carbon spectrum signal integral intensity. The method has the following advantages: the structure information can be directly obtained through determining the glucose polymer by a nuclear magnetic resonance technology, so the limitations of traditional chemical methods are broken; and the proton signal integral of glycosides in C1 of a glucose residue in alpha-1,6 linkage is calculated to obtain the branching degree, or the C6 signal integral of the glucose residue in the alpha-1,6 linkage is calculated to obtain the branching degree, so the determination precision is effectively improved, andthe determination step is simplified.

Description

Technical field: [0001] The invention relates to a method for measuring the branching degree of glucose polymers, in particular to a method for measuring the branching degree of glucose polymers by nuclear magnetic resonance. Background technique: [0002] Starch is a mixture of biological macromolecular polysaccharides. Natural starch generally contains two components: amylose and amylopectin. , 6 connections, there are many existing literature reports on the methods of starch structure determination, which can be roughly divided into two categories: traditional chemical methods and spectroscopy methods. [0003] Traditional chemical methods generally include hydrolysis, oxidation, methylation, smith degradation, etc. Spectroscopy methods are roughly divided into: ultraviolet spectrophotometry, infrared spectroscopy, etc. The structural analysis of starch by traditional chemical methods, especially the determination of the starch linkage method, is cumbersome and difficult...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N24/08
CPCG01N24/08
Inventor 王艺鸣王文彦孙建
Owner 青岛力腾医药科技有限公司
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