Method for preparing water soluble chitosan oligosaccharide from squid sheath and bioactivity of chitosan oligosaccharide

A water-soluble chitosan oligosaccharide and squid sheath technology, which is applied in the preparation of sugar derivatives, sugar derivatives, sugar derivatives, etc., can solve the problems of low yield, corrosion equipment, environmental pollution, etc.

Inactive Publication Date: 2013-01-16
ZHEJIANG UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

With the development of medicine and food industry, the demand for chitosan oligosaccharides is increasing day by day. However, the traditional process of hydrolyzing chitosan to

Method used

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  • Method for preparing water soluble chitosan oligosaccharide from squid sheath and bioactivity of chitosan oligosaccharide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Crush squid sheath into powder, weigh 400g of squid sheath powder, add 5600mL of 8% HCl solution, decalcify at room temperature for 30mmin, observe no bubbles, and wash until neutral. Then add 4000mL of 10% NaOH solution, deproteinize in a water bath at 100°C for 1 hour, filter and wash until neutral, dry at 60°C to obtain β-chitin, and crush it for use. Take 200g of β-chitin and add 2000mL of 50% HCl solution, ultrasonically react at 80°C for 2h, and ultrasonic frequency is 25KHz. After the reaction, filter with suction, and wash the filter cake to neutral chitosan. Take 40g chitosan, add 90mL 30% H 2 o 2 , and then add 810mL of distilled water to make H 2 o 2 The concentration is 3%, and it is reacted at 65°C for 4 hours under the assistance of ultrasonic waves, and the frequency is 40KHz. After the reaction is completed, it is adjusted to neutrality with NaOH, distilled under reduced pressure, so that the volume is concentrated to 1 / 10 of the original volume, and...

Embodiment 2

[0025] Crush the squid sheath into powder, weigh 400g of squid sheath powder, add 5600mL of 8% HCl solution, decalcify at room temperature for 30min, observe that no bubbles are generated, and wash until neutral. Then add 4000mL of 10% NaOH solution, deproteinize in a water bath at 100°C for 1 hour, filter and wash until neutral, dry at 60°C to obtain β-chitin, and crush it for use. Take 200g of β-chitin and add 2000mL of 50% HCl solution, ultrasonically react at 80°C for 2h, and ultrasonic frequency is 25KHz. After the reaction, filter with suction, and wash the filter cake to neutral chitosan. Take 40g chitosan, add 270mL 30% H 2 o 2 , and then add 630mL of distilled water to make H 2 o 2 The concentration is 9%, and the reaction is 4h at 65°C under the assistance of ultrasonic waves, and the frequency is 40KHz. After the reaction is completed, adjust to neutral with NaOH, distill under reduced pressure to make the volume concentrated to 1 / 10 of the original volume, and ...

Embodiment 3

[0027]Crush the squid sheath into powder, weigh 400g of squid sheath powder, add 5600mL of 8% HCl solution, decalcify at room temperature for 30mmin, observe that no bubbles are generated, and wash until neutral. Then add 4000mL of 10% NaOH solution, deproteinize in a water bath at 100°C for 1 hour, filter and wash until neutral, dry at 60°C to obtain β-chitin, and crush it for use. Take 200g of β-chitin and add 2000mL of 50% HCl solution, ultrasonically react at 80°C for 2h, and ultrasonic frequency is 25KHz. After the reaction, filter with suction, and wash the filter cake to neutral chitosan. Take 40g chitosan, add 180mL 30% H 2 o 2 , and then add 720mL of distilled water to make H 2 o 2 The concentration is 6%, and it is reacted at 45°C for 3 hours under the assistance of ultrasonic waves, and the frequency is 40KHz. After the reaction is completed, it is adjusted to neutrality with NaOH, distilled under reduced pressure, so that the volume is concentrated to 1 / 10 of t...

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Abstract

The invention discloses a method for preparing water soluble chitosan oligosaccharide from squid sheath. The method is characterized by comprising the following steps of: crushing the squid sheath, adding 6 to 9 percent HCl solution, ensuring that a material/solution (w/v) ratio is 1:14, decalcifying for 20 to 60 minutes, washing to neutrality, adding 10 percent NaOH solution, ensuring that a material/solution (w/v) ratio is 1:10, removing protein, filtering and washing to neutrality, and drying to obtain beta-chitin; adding 30 to 50 percent NaOH solution into the beta-chitin, ensuring that a material/solution ratio (w/v) is 1:10, performing ultrasonic bath reaction at the temperature of between 70 and 100DEG C for 2 to 4 hours, filtering, washing to neutrality, and drying to obtain chitosan; and adding 3 to 12 percent H2O2 into the chitosan, ensuring that a material/solution ratio (m/v) is 1:15-1:25, reacting at the temperature of between 45 and 75DEG C for 2 to 5 hours in the assistance of ultrasonic waves, concentrating filtrate, adding ethanol in an amount which is 3 to 5 times volume of the concentrated filtrate, precipitating and filtering a product, and drying to obtain the chitosan oligosaccharide, wherein the chitosan oligosaccharide has the molecular weight of less than 1*10<4>Da, the DPPH free radical removing capacity (EC50) of between 0.3 and 1.3mg/mL and the cholic acid combining capacity of between 20.47 and 63.53mg/g. The invention provides technical support for comprehensively utilizing leftovers, namely the squid sheath in aquatic product processing and industrially producing the water soluble chitosan oligosaccharide.

Description

technical field [0001] The invention relates to a method for preparing water-soluble chitosan oligosaccharide by using squid sheath and the biological activity of chitosan oligosaccharide. Background technique [0002] Chitin, also known as chitin, chitin, etc., widely exists in the shells of arthropods (such as shrimp, crab, squid, etc.) in nature, and also exists in lower animals such as fungi, insects, and algae. In the cell wall, it is the largest nitrogen-containing natural polymer compound on the earth after cellulose. The scientific name of chitin is β-1,4-poly-N-acetyl-D-glucosamine, and its molecular formula is (C 8 h 13 NO 5 )n. Chitosan (chitosan) is the product of deacetylation of chitin, also known as chitosan, deacetylated chitin, etc., its scientific name is β-1,4-poly-D-glucosamine, and its molecular formula is (C 6 h 11 NO 4 )n. Chitosan is white or off-white, amorphous, translucent, pearlescent flaky or powdery solid, insoluble in water and alkaline...

Claims

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Application Information

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IPC IPC(8): C08B37/08C07H5/06C07H1/00A61P39/06A61P1/16
Inventor 毛建卫黄俊刘士旺吴元锋平丽娟王永江许茂乾
Owner ZHEJIANG UNIVERSITY OF SCIENCE AND TECHNOLOGY
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