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A Calculation Method of Infrared Fitting Calculation of Chitosan Deacetylation Degree

A calculation method and technology of deacetylation degree, which are used in instruments, measuring devices, scientific instruments, etc.

Active Publication Date: 2021-09-10
DALIAN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, for the enterprise quality inspection department 1 H NMR spectroscopy is not a cheap test

Method used

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  • A Calculation Method of Infrared Fitting Calculation of Chitosan Deacetylation Degree
  • A Calculation Method of Infrared Fitting Calculation of Chitosan Deacetylation Degree
  • A Calculation Method of Infrared Fitting Calculation of Chitosan Deacetylation Degree

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Infrared fitting calculation method to calculate the degree of deacetylation of chitosan:

[0038] (1) Take by weighing 0.0011g of chitosan to be measured (degree of deacetylation, DD 93.8%) and 0.1100g of potassium bromide powder in an amber mortar, both are ground to fine;

[0039] (2) Send the mixed powder obtained through grinding in step (1) to a tablet machine for tableting, and press for 5 minutes under a pressure of 50 MPa;

[0040] (3) Utilize the Fourier transform infrared instrument to the tablet that obtains in step (2) at 400-4000cm -1 Carry out scanning test in the range of wave number, obtain absorbance spectrogram, promptly obtain the chitosan infrared spectrogram to be tested;

[0041] (4) carry out baseline correction and smoothing processing in the infrared spectrogram data that obtains in step (3) in OMNIC software; Wherein, baseline correction can adopt automatic baseline correction, and the smoothing point number of smoothing processing is 25 poin...

Embodiment 2

[0060] According to the infrared fitting calculation method described in the steps (1)~(6) of embodiment 1, calculate the degree of deacetylation of chitosan to be measured, wherein the steps different from the present embodiment in embodiment 1 are:

[0061] In step (1), weigh 0.0013g of chitosan to be tested (degree of deacetylation, DD 86.4%) and 0.1300g of potassium bromide powder in an amber mortar, and grind the two until fine.

[0062] The fitting peak I-VI obtained in step (5), the peak area percentage A of the fitting peak I-VI Ⅰ -A Ⅵ followed by A Ⅰ =5.3, A Ⅱ = 44.1, A Ⅲ =0.7,A Ⅳ =16.0,A Ⅴ =1.0,A Ⅵ = 0.8.

[0063] As a verification example of the results obtained with the infrared fitting calculation method of the present embodiment, the existing ultraviolet spectrometry and potentiometric titration are used to measure the deacetylation degree of the same chitosan (deacetylation degree, DD 86.4%) , the specific assay method is the same as in Example 1.

[00...

Embodiment 3

[0066] According to the infrared fitting calculation method described in the steps (1)-(6) of embodiment 1, calculate the degree of deacetylation of chitosan to be measured, wherein the steps that embodiment 1 is different from the present embodiment are:

[0067] In step (1), weigh 0.0014g of chitosan (degree of deacetylation, DD 75.9%) and 0.1400g of potassium bromide powder in an amber mortar, and grind the two until fine.

[0068] The fitting peaks I~VI obtained in step (5), the peak area percentage A of the fitting peaks I~VI Ⅰ -A Ⅵ followed by A Ⅰ =9.6,A Ⅱ = 41.1, A Ⅲ =0.3,A Ⅳ = 0, A Ⅴ =1.1,A Ⅵ = 12.5.

[0069] As a verification example of the results obtained with the infrared fitting calculation method of the present embodiment, the existing ultraviolet spectrometry and potentiometric titration are used to measure the deacetylation degree of the same chitosan (deacetylation degree, DD 86.4%) , the specific assay method is the same as in Example 1.

[0070] The...

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Abstract

The invention discloses a calculation method for calculating the deacetylation degree of chitosan by infrared fitting. After correcting the infrared spectrogram curve of the chitosan to be measured, carry out peak fitting according to the wave number of different functional group positions, and account for 3700-3000cm by the area of ​​each fitting peak ‑1 The deacetylation degree of chitosan can be obtained by simple addition, subtraction, multiplication and division of the percentage of chitosan infrared spectrum peak area to be measured within the range. Adopt the method of the present invention to divide the peak to fit the infrared spectrum of chitosan, can correctly reduce each functional group of chitosan at 3700-3000cm ‑1 The independent vibration of the chitosan to be tested can be obtained to obtain the number of hydroxyl groups and amino groups contained in the chitosan to be tested, and finally the degree of deacetylation of the chitosan to be tested can be calculated. The calculation formula of the invention is simple, the result is accurate, the deacetylation degree of the chitosan can be calculated and checked, and the invention can be applied to the quality inspection department to quickly test samples.

Description

technical field [0001] The invention belongs to the field of testing methods for the degree of deacetylation of chitosan, and relates to a method for calculating the degree of deacetylation of chitosan through infrared fitting. Background technique [0002] Chitosan (Chitosan, abbreviated as CS), as a natural polymer material, is famous for its excellent antibacterial, non-toxic, hemostatic and biocompatibility. It can be prepared from chitin by deacetylation reaction. Chitin is reacted at 100° C. under 40-50% NaOH solution for different hours to obtain chitosan with a deacetylation degree of 49-100%. Since the solubility of chitosan is affected by the degree of deacetylation, it directly affects the application performance of chitosan in many fields. Therefore, the detection of the degree of deacetylation is a process that must be measured in the quality inspection of every manufacturer, and it is also an important chemical parameter that must be provided when the article...

Claims

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Application Information

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IPC IPC(8): G01N21/3563
CPCG01N21/3563G01N2021/3572G01N2021/3595
Inventor 郭静陈杰曹政宫玉梅
Owner DALIAN POLYTECHNIC UNIVERSITY
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