Method for determining substitution degree of hydroxypropyl chitosan

A technology of hydroxypropyl chitosan and chitosan, which is applied in the direction of color/spectral characteristic measurement, etc., can solve problems such as difficulty in determining the degree of substitution of hydroxypropyl chitosan, and unseen problems

Active Publication Date: 2015-12-02
QINGDAO UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] However, the research on hydroxypropyl chitosan has been started since the 1980s at home and abroad. Researchers generally use its infrared absorption spectrum as one of the methods for structural characterization, but so far, no use of this method has been used to determine hydroxypropyl chitosan. Related reports on degree of substitution of chitosan
The reason is that, on the one hand, the extremely small amount of impurities in the hydroxypropyl chitosan sample can make its infrared spectrum "clearly discern the details" and appear, and directly affect the peak shape and peak position changes of the characteristic peaks (Zhang Yongqin, Zhang Kun. The effect of separation and purification methods on the determination of the structure and degree of substitution of hydroxypropyl chitosan. Journal of Qingdao University of Science and Technology, 2015, 36(3):251-254); on the other hand, hydroxypropylation itself will also make it The characteristic peaks overlap, deform, migrate, etc., and it is difficult to find a constant characteristic peak of a certain structure as a reference peak for the calculation of the degree of substitution

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  • Method for determining substitution degree of hydroxypropyl chitosan
  • Method for determining substitution degree of hydroxypropyl chitosan
  • Method for determining substitution degree of hydroxypropyl chitosan

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Reagents: KBr is optically pure, and acetanilide is a standard substance, both from Sinopharm Reagent Co., Ltd. Chitosan, derived from Laixi Haili Bioengineering Co., Ltd.; hydroxypropyl chitosan, using Chitosan No. 0 as raw material, reacts differently with propylene oxide at 45-60°C under alkaline conditions Time, hydroxypropyl chitosan No. 1-No. 4 with different degrees of substitution purified by dealkalization.

[0036] Instrument: the present invention is applicable to various Fourier transform infrared spectrometers, and instrument used in the present invention is the Fourier transform infrared spectrometer TENSOR27 of German Bruker (Bruker) company; The degree of acetylation and the degree of substitution of hydroxypropyl chitosan were completed in the testing center (national open laboratory) of the Institute of Bioenergy of the Chinese Academy of Sciences certified by the National Bureau of Metrology, and the instrument used was the VarioELcube elemental analy...

Embodiment 2

[0052] The hydroxypropyl chitosan samples A, B, C, D, E, and F to be tested were all purified by hydroxypropylation and dealkalization. The degree of deacetylation of the raw material chitosan is 92.2%, 93.8%, 94.4%, 95.1%, 96.3%, 97.6%. Compared with the raw chitosan (95.1%) of the hydroxypropyl chitosan sample used to establish the linear regression equation, the deacetylation degree differs by up to 3.05%. The hydroxypropyl chitosan to be tested dried according to the method (1) is passed through the Fourier transform infrared spectrometer according to the step (2a) and background detection and background processing are performed, so as to obtain an infrared absorption spectrum. According to the method of step (2)b, in the OPUS software, select the C baseline integration method to measure the methyl characteristic peak 1460-1456cm -1 The absorbance value A1 of the peak height, with the whole waveform 1530-1215cm -1 The line connecting the troughs is the baseline BL1, and ...

Embodiment 3

[0056] The dealkalization purification method of hydroxypropyl chitosan

[0057] After the raw material chitosan undergoes hydroxypropylation reaction with propylene oxide under alkaline conditions, it needs to be purified by dealkalization. The de-alkalization purification method of the sample includes the de-alkalization method of alcohol washing, ketone precipitation, dialysis and partial neutralization ultrafiltration de-alkalization method.

[0058] In the alcohol washing ketone precipitation dialysis dealkalization method, firstly, the product mixture is suction-filtered to remove the solvent and residual alkali. Add water to dissolve the crude product after suction filtration, filter, add ethanol to the filtrate to make it contain 75% ethanol, add acetone while stirring to precipitate the swollen chitosan, filter, and add the precipitate to 75% ethanol , and so on, until the ethanol aqueous solution of hydroxypropyl chitosan is neutral, then precipitate it with acetone...

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Abstract

The invention discloses a method for determining the substitution degree of hydroxypropyl chitosan. The method comprises the steps that 1, a hydroxypropyl chitosan sample is dried; 2, a detection model is established, and the establishment process comprises the steps that a, an infrared absorption spectrum of the sample is obtained through an infrared absorption spectrometer; b, the specific value X of an absorbance value A1 of the area of a methyl characteristic peak ranging from 1460 cm<-1> to 1456 cm<-1> to an absorbance value A2 of the peak height of a characteristic peak, ranging from 1602 cm<-1> to 1596 cm<-1>, of amino on the C2 position is determined; c, the substitution degree Y of the hydroxypropyl chitosan sample is determined through a standard method; d, a good linear regression model Y=kX + b is established by using Y on X, and therefore specific values of k and b in the model are obtained; 3, the specific value X, obtained through the infrared absorption spectrum, of the sample to be determined is substituted into the linear regression model, and then the substitution degree Y can be obtained through calculation. The method is simple, convenient, rapid and accurate, and precise weighing and sample dissolution are not needed.

Description

technical field [0001] The invention belongs to the field of research and application of detection methods for the degree of substitution of hydroxypropyl chitosan, and relates to a method for determining the degree of substitution of hydroxypropyl chitosan, in particular to an infrared absorption spectrometry method for determining the degree of substitution of hydroxypropyl chitosan. degree method. Background technique [0002] Chitosan has good biocompatibility, biodegradability, stability, and safety, but its water solubility is poor, and it can only be dissolved in acidic media, and chitosan is hydroxypropylated to form a hydroxypropyl shell Glycans can improve their solubility, thereby greatly broadening their application fields and development process. Studies have shown that hydroxypropyl chitosan has solubility, hygroscopicity, moisturizing properties, film-forming properties, foaming properties, free radical scavenging, antibacterial properties, and adsorption pro...

Claims

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Application Information

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IPC IPC(8): G01N21/35
Inventor 张永勤张捷张坤武玉民
Owner QINGDAO UNIV OF SCI & TECH
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