Preparation method of water-soluble chitosan-oligosaccharide
A technology of chitooligosaccharide and water-solubility, applied in the field of preparation of chitooligosaccharide, can solve the problems of low molecular weight, influence product quality, poor physiological activity of the product, etc., and achieve the purpose of reducing production requirements and production costs, and facilitating purification and separation. Effect
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Embodiment 1
[0023] Embodiment 1: Accurately weigh 10.0 g of chitosan with a degree of deacetylation of 70%, and dissolve it in 0.5% acetic acid solution to prepare a 2% (w / v) chitosan acetic acid solution. The temperature was raised to 55°C, and the molar ratio of chitosan to hydrogen peroxide was 1:1.5, and 2% H was added. 2 o 2 Solution, pH 5.5, after continuous stirring for 70min and hydrolysis, 3ml of hydrolyzate was added to 2ml of 4mol / L NaOH solution without flocculent precipitation. Manganese terminates the reaction until no bubbles are generated, and the reaction solution is filtered to remove MnO 2 (MnO 2 collected and recycled), and the filtrate was spray-dried to obtain a weight-average molecular weight of 80,000 completely water-soluble chitooligosaccharides.
[0024] where, 2% H 2 o 2 The solution is H per 100 ml of water 2 o 2 The mass is 2g.
Embodiment 2
[0025] Embodiment 2: Accurately weigh 10.0 g of chitosan with a degree of deacetylation of 85%, and dissolve it with a 1.0% acetic acid solution to prepare a 3% (w / v) chitosan acetic acid solution. The temperature was raised to 60°C, and the molar ratio of chitosan to hydrogen peroxide was 1:2.0, and 2% H was added. 2 o 2 solution, pH 6.0, after continuous stirring for 1 hour for hydrolysis, the hydrolyzate was added to 4mol / L NaOH solution without flocculent precipitation. Pure manganese dioxide terminates the reaction until no bubbles are generated, and the reaction solution is filtered to remove MnO 2 (MnO 2 collected and recycled), the filtrate was collected and spray-dried to obtain a fully water-soluble chitooligosaccharide with a weight average molecular weight of 10,000.
Embodiment 3
[0026] Embodiment 3: Accurately weigh 10.0 g of chitosan with a degree of deacetylation of 95%, and dissolve it with a 1.5% acetic acid solution to prepare a 4% (w / v) chitosan acetic acid solution. The temperature was raised to 65°C, and the molar ratio of chitosan to hydrogen peroxide was 1:2.5, and 2% H was added. 2 o 2 solution, the pH was adjusted to 6.5, and after continuous stirring for 1 hour for hydrolysis, the hydrolyzate was added to 4mol / L NaOH solution without flocculent precipitation. High-purity manganese dioxide terminates the reaction until no bubbles are generated, and the reaction solution is filtered to remove MnO 2 (MnO 2 collected and recycled), and the filtrate was collected to obtain completely water-soluble chitooligosaccharides with a weight-average molecular weight of 986 through a spray-drying method.
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