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Method for separation and purification of thermo-sensitive hydroxybutyl chitosan by phase transformation

A temperature-sensitive hydroxybutyl chitosan separation and purification technology is applied in the field of separation and purification of temperature-sensitive hydroxybutyl chitosan, which can solve the problems of limitation and no purification of temperature-sensitive hydroxybutyl chitosan, etc. To achieve the effect of increasing the molecular weight

Active Publication Date: 2015-07-08
SHANGHAI QISHENG BIOLOGICAL PREPARATION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the industrial transformation process of hydroxybutyl chitosan, the safety of the product is one of the most important control indicators, and the traditional process is to separate and purify it to remove toxic impurities in the product. The most commonly used method is alcohol grading Precipitation, and the solubility of hydroxybutyl chitosan in alcohol at low concentrations greatly increases the application of this method, so providing a scientific and complete separation and purification scheme for the above problems is the first to bear the brunt of the industrial transformation of hydroxybutyl chitosan The problem
However, there is no invention patent specifically for the purification of temperature-sensitive hydroxybutyl chitosan and its derivatives in the domestic published or authorized patents

Method used

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  • Method for separation and purification of thermo-sensitive hydroxybutyl chitosan by phase transformation
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  • Method for separation and purification of thermo-sensitive hydroxybutyl chitosan by phase transformation

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Experimental program
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Effect test

Embodiment 1

[0026] Concentrations of 2%, 10% and 20% sodium chloride aqueous solution and 2% thermosensitive hydroxybutyl chitosan aqueous solution were prepared respectively. First add 2% aqueous sodium chloride solution to 500ml of thermosensitive hydroxybutyl chitosan aqueous solution in a stirring state until white precipitates are separated out. After filtering the solution, add 500ml of 10% aqueous sodium chloride solution and stir fully. After the solution was filtered off, 500 ml of 20% sodium chloride aqueous solution was added, stirred thoroughly, and after the solution was filtered off, a white precipitate crude product was obtained.

[0027] The precipitate was washed with 70%, 80%, 90% and 100% acetone 500ml to desalt in turn, and finally a white precipitate was obtained. After the precipitate was vacuum-dried at 40°C, the refined pure product of temperature-sensitive hydroxybutyl chitosan was obtained. 7.4g.

[0028]

Embodiment 2

[0030] The concentrations were 4%, 15% and 20% sodium chloride aqueous solution, and 1% thermosensitive hydroxybutyl chitosan aqueous solution. First add 4% aqueous sodium chloride solution to 500ml of thermosensitive hydroxybutyl chitosan aqueous solution in a stirring state until white precipitates are separated out. After filtering the solution, add 500ml of 15% aqueous sodium chloride solution and stir fully. After the solution was filtered off, 500 ml of 20% sodium chloride aqueous solution was added, stirred thoroughly, and after the solution was filtered off, a white precipitate crude product was obtained.

[0031] The precipitate was washed with 70%, 80%, 90% and 100% acetone 500ml to desalt in turn, and finally a white precipitate was obtained. After the precipitate was vacuum-dried at 40°C, the refined pure product of temperature-sensitive hydroxybutyl chitosan was obtained. 3.2g.

[0032]

Embodiment 3

[0034] The concentrations were 5%, 15% and 25% sodium chloride aqueous solution and 0.5% thermosensitive hydroxybutyl chitosan aqueous solution respectively. First add 5% aqueous sodium chloride solution to 500ml of thermosensitive hydroxybutyl chitosan aqueous solution in a stirring state until white precipitates are separated out. After filtering the solution, add 500ml of 15% aqueous sodium chloride solution and stir fully. After filtering off the solution, add 500ml of 25% sodium chloride aqueous solution, stir well, and after filtering off the solution, a white precipitate crude product is obtained.

[0035] The precipitate was washed with 500ml of 70%, 80%, 90% and 100% ethanol in order to remove salt, and finally a white precipitate was obtained. The precipitate was vacuum-dried at 40°C to obtain the refined pure product of temperature-sensitive hydroxybutyl chitosan 1.6 g.

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Abstract

The invention provides a method for separation and purification of thermo-sensitive hydroxybutyl chitosan by a phase transformation principle. The method mainly utilizes a mechanism that thermo-sensitive hydroxybutyl chitosan can generate sol-gel phase transformation along with increase of ionic strength; based on the above mechanism, salt solutions with different concentration gradients are utilized, a certain concentration of thermo-sensitive hydroxybutyl chitosan is subjected to fractional precipitation, then gradient elution is carried out by utilizing organic solvents with different concentration gradients, and finally, 40 DEG C vacuum drying is carried out to obtained a purified thermo-sensitive hydroxybutyl chitosan dry powder. Through the above method, any damage to a chemical structure of the thermo-sensitive hydroxybutyl chitosan does not generated, at the same time, impurities and small molecular fragments in the solutions are effectively removed, the molecular weight and molecular weight distribution of the thermo-sensitive hydroxybutyl chitosan are improved, an ideal separation and purification effect is obtained, the problem that the thermo-sensitive hydroxybutyl chitosan cannot be purified by concentrating precipitation is solved ultimately, and large-scale production and quality control becomes possible.

Description

technical field [0001] The invention relates to a separation and purification method of temperature-sensitive hydroxybutyl chitosan, which is suitable for basic research and large-scale production of temperature-sensitive hydroxybutyl chitosan derivatives, and the use of the method gets rid of the traditional The disadvantage of ineffective precipitation by the concentrated precipitation method makes the large-scale production and quality control of thermosensitive hydroxybutyl chitosan possible. Background technique [0002] Thermosensitive chitosan is a class of chitosan derivatives that can respond intelligently to changes in external temperature. Its main feature is that it is a flowing liquid at low temperature, and when the temperature rises, the temperature Sensitive hydroxybutyl chitosan can undergo intelligent phase transition and transform into a non-flowing gel; the temperature at which the phase transition occurs is called the lowest critical solution temperature...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08
Inventor 魏长征奚宏伟侯春林
Owner SHANGHAI QISHENG BIOLOGICAL PREPARATION CO LTD
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