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Preparation method of chitosan microspheres

A technology of chitosan microspheres and carapaces, which is applied in the field of preparation of chitosan microspheres, can solve the problems of increased drug levels, insufficient therapeutic effects, and reductions, and achieve reduced degradation, high deacetylation, and enzymatic hydrolysis high efficiency effect

Active Publication Date: 2017-01-04
上海丽珠制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Through the traditional way of administration, most of the drug ingredients are released very quickly, causing the drug level in the body to rise rapidly, reach the peak and then decrease rapidly
For drugs, their effects are closely related to the concentration of the drug in the serum, and the drastic fluctuations often cause unacceptable side effects at the peak, and then insufficient therapeutic effect due to the low concentration of the drug in the serum

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Decalcification: After crushing 10g of insect carapaces, place them in 200g of dilute acid with a mass concentration of 10% and soak for 4 hours at 50°C, filter, wash the filter cake with water for 3-5 times and dry to obtain 7.2g of decalcified Product A;

[0034] (2) Deproteinization: put 7.2g decalcification product A, 0.09g trypsin, 0.09g papain, 0.18g alkaline lipase and 144g water in a three-necked flask, control the pH of the reaction solution to 7.5, and stir at 40°C After hydrolysis for 3 hours, filter, wash and dry the filter cake to obtain 4.3 g of deproteinized product B;

[0035] (3) Purification: 4.3g of deproteinized product B, 28g of hexanoic acid, 22g of oxalic acid, 14g of pyridine and 0.43g of NaCl were stirred and dissolved at 60°C for 3 hours, then filtered, and the filtrate was dried under reduced pressure to remove the solvent, and then passed through NaCl was removed by washing with water, and 3.2 g of chitin was obtained by drying. The HPLC...

Embodiment 2

[0042] (1) Decalcification: After crushing 10g of insect carapaces, place them in 250g of dilute acid with a mass concentration of 15% and soak for 6 hours at 30°C, filter, wash the filter cake with water for 3-5 times and dry to obtain 7.8g of decalcified Product A;

[0043] (2) Deproteinization: put 7.8g decalcified product A, 0.12g trypsin, 0.12g papain, 0.24g alkaline lipase and 78g water in a three-necked flask, control the pH of the reaction solution to 8, and stir at 50°C After hydrolysis for 2.5 hours, filter, wash and dry the filter cake to obtain 5.1 g of deproteinized product B;

[0044] (3) Purification: 5.1g deproteinized product B, 40g hexanoic acid, 32g oxalic acid, 20g pyridine and 1g MgSO 4 , stirred and dissolved at 70°C for 2 hours, filtered, and the filtrate was dried under reduced pressure to remove the solvent, and then washed with water to remove MgSO 4 , dried to obtain 3.8g chitin, the HPLC purity was 93.8%, the recovery rate was 35.6%, and the ash c...

Embodiment 3

[0050] (1) Decalcification: After crushing 10g of insect carapaces, put them in 300g of dilute acid with a mass concentration of 20% and soak for 5 hours at 40°C, filter, wash the filter cake with water for 3-5 times and dry to obtain 6.9g of decalcified Product A;

[0051] (2) Deproteinization: put 6.9g decalcification product A, 0.14g trypsin, 0.14g papain, 0.28g alkaline lipase and water in a three-necked flask, control the pH of the reaction solution to 8.5, stir and hydrolyze at 55°C After 2 hours, filter, take the filter cake and wash and dry to obtain 4.6g of deproteinized product B;

[0052] (3) Purification: 4.6g deproteinized product B, 40g hexanoic acid, 32g oxalic acid, 20g pyridine and 1.4g Na 2 SO 4 , stirred and dissolved at 80°C for 1 hour, filtered, and the filtrate was dried under reduced pressure to remove the solvent, and then washed with water to remove Na 2 SO 4 , dried to obtain 3.5g of chitin, the HPLC purity was 93.1%, the recovery rate was 32.6%, ...

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Abstract

The invention provides a preparation method of chitosan microspheres. The preparation method comprises steps as follows: calcium removal with insect carapace diluted acid, deproteinization through compound enzymes, dissolution and purification of a mixed solvent, deacetylation of weak base through ultraviolet light and emulsification crosslinking, and the chitosan microspheres are prepared with the method. Chitosan prepared with the method has high purity, high degree of deacetylation and large molecular weight, the size of the chitosan microspheres prepared from chitosan ranges from 210 mu m to 400 mu m, the deviation is lower than 15%, and the application requirement of the chitosan microspheres in interventional therapy is met.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of chitosan microspheres. Background technique [0002] Chitosan, also known as deacetylated chitin, soluble chitin and polyglucosamine, its chemical name is β-(1→4)-2-amino-2-deoxy-D-glucose, after chitin is treated with concentrated alkali The product obtained by removing the acetyl group. Chitosan has excellent biocompatibility and low toxicity, and can be dissolved and metabolized by lytic enzymes in the human body. [0003] Through the traditional way of administration, most of the drug ingredients are released very quickly, causing the drug level in the body to rise rapidly, reach a peak and then decrease rapidly. As for the drug, its effect is closely related to the concentration of the drug in the serum, and violent fluctuations often cause unacceptable side effects at the peak, and then insufficient therapeutic effect due to...

Claims

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Application Information

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IPC IPC(8): C08J3/24C08J3/12C08J3/16C08B37/08A61K47/36C08L5/08
CPCA61K47/36C08B37/0003C08B37/003C08J3/12C08J3/16C08J3/24C08J2305/08
Inventor 倪协照
Owner 上海丽珠制药有限公司
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