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Photo-initiated cross-linked polyvinyl alcohol drug-loaded embolism microsphere and preparation method thereof

A technology for cross-linking polyvinyl alcohol and polyvinyl alcohol is applied in the field of medical materials to achieve the effects of good spheroidization, simple equipment and better drug-carrying effect.

Active Publication Date: 2022-03-01
SHANGHAI HUIHE HEALTHCARE TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method uses potassium persulfate and tetraethylethylenediamine which are more toxic as thermal initiators, and needs to react at 55°C for 3 hours

Method used

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  • Photo-initiated cross-linked polyvinyl alcohol drug-loaded embolism microsphere and preparation method thereof
  • Photo-initiated cross-linked polyvinyl alcohol drug-loaded embolism microsphere and preparation method thereof
  • Photo-initiated cross-linked polyvinyl alcohol drug-loaded embolism microsphere and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0035] S1. Synthesis of photocrosslinkable polyvinyl alcohol intermediates by acid catalysis

[0036] 100 g of purified water and 12 g of polyvinyl alcohol with a weight average molecular weight of 67,000 were added to the reaction flask, and heated to 95° C. to completely dissolve the polyvinyl alcohol. Add 1.5g N-(2,2-dimethoxyethyl)-2-acrylamide and 20mL concentrated hydrochloric acid, and react at 30°C for 4 hours. The pH was adjusted to 7. Finally, the solution was concentrated to a viscosity of 1800 cps to obtain about 40 g of the microsphere intermediate.

[0037] S2. Preparation of polyvinyl alcohol embolization microspheres by photoinitiated crosslinking

[0038] Add 9g microsphere intermediates, 0.6g 2-acrylamide-2-methylpropanesulfonic acid sodium salt, 0.09g 2-hydroxyl-2-methyl-1-[4-( 2-hydroxyethoxy)phenyl]-1-propanone, then add 5mL water to dissolve completely. Then add 60mL of butyl acetate and 0.4g of cellulose acetate butyrate, stir to form a suspension, a...

Embodiment 2

[0040] S1. Synthesis of photocrosslinkable polyvinyl alcohol intermediates by acid catalysis

[0041] Add 1,000 g of purified water and 300 g of polyvinyl alcohol with a weight average molecular weight of 35,000 into the reaction flask, and heat to 85° C. to completely dissolve the polyvinyl alcohol. Add 100g N-(2,2-dimethoxyethyl)-2-acrylamide and 150mL concentrated hydrochloric acid, and react at 20°C for 5 hours. After the reaction, adjust the pH of the reaction system with 1mol / L sodium hydroxide solution Adjust to 7.5. Finally, the solution was concentrated to a viscosity of 2000 cps to obtain 900 g of microsphere intermediates.

[0042]S2. Preparation of polyvinyl alcohol embolization microspheres by photoinitiated crosslinking

[0043] Add 100g microsphere intermediate, 20g 2-acrylamide-2-methylpropanesulfonic acid sodium salt, 2g 2-hydroxyl-2-methyl-1-[4-(2- Hydroxyethoxy)phenyl]-1-propanone, 0.3g N-vinylpyrrolidone, and then add 20mL water to dissolve completely. ...

Embodiment 3

[0045] S1. Synthesis of photocrosslinkable polyvinyl alcohol intermediates by base catalysis

[0046] Add 600 mL of dimethyl sulfoxide and 100 g of polyvinyl alcohol with a weight average molecular weight of 78,000 to the reaction flask, and heat to 80° C. to completely dissolve the polyvinyl alcohol. 5 g of glycidyl methacrylate and 10 mL of tetramethylethylenediamine were added, and the reaction was stirred at 60° C. for 5 hours. After the reaction is finished, ethanol as a precipitating agent is added to the reaction system to precipitate the modified polyvinyl alcohol. The modified polyvinyl alcohol was obtained after filtration, and redissolved to form a 23% polyvinyl alcohol aqueous solution as a photocrosslinkable polyvinyl alcohol intermediate.

[0047] S2. Preparation of polyvinyl alcohol embolization microspheres by photoinitiated crosslinking

[0048] 20g of the above-mentioned polyvinyl alcohol intermediate, 0.34g of 2-acrylamide-2-methylpropanesulfonic acid sodi...

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Abstract

The invention provides a photo-initiated cross-linked polyvinyl alcohol drug-loaded embolism microsphere and a preparation method thereof, and belongs to the technical field of medical materials. Comprising the following steps: S1, reacting polyvinyl alcohol through an acid catalysis method or a base catalysis method to obtain a photo-crosslinkable polyvinyl alcohol intermediate; s2, dissolving the photo-crosslinkable polyvinyl alcohol intermediate, 2-acrylamide-2-methyl propanesulfonic acid sodium salt and a water-soluble photoinitiator in water under a dark condition, adding the solution into a mixed solution of butyl acetate and cellulose acetate butyrate, stirring to form a suspension, initiating a cross-linking reaction under irradiation of a light source, washing after the reaction is finished, and drying to obtain the photocrosslinkable polyvinyl alcohol. The photo-initiated cross-linked polyvinyl alcohol drug-loaded embolism microspheres are obtained. According to the invention, the polymerization reaction time and energy consumption can be reduced, the reaction can be completed within only 5 minutes to 2 hours, the reaction can be carried out at room temperature, the environment-friendly photoinitiator is used, and the method is more suitable for large-scale production.

Description

technical field [0001] The invention relates to the technical field of medical materials, in particular to a photoinitiated cross-linked polyvinyl alcohol drug-loaded embolic microsphere and a preparation method thereof. Background technique [0002] Embolization microspheres have become an important clinical treatment for tumor diseases, especially liver tumors. The microspheres can be selectively and controlledly injected into the blood supply vessels of the tumor body through the catheter to achieve occlusion and block the blood supply of the tumor. At the same time, the microspheres can also be loaded with chemotherapeutic drugs, thus organically combining arterial infusion chemotherapy and local arterial embolization, embolizing tumor blood vessels and blocking tumor blood supply at different levels, and slowly releasing chemotherapeutic drugs through microspheres. Longer time, higher drug concentration of local chemotherapy, and can significantly reduce the concentrat...

Claims

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Application Information

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IPC IPC(8): A61L24/06A61L24/00C08F261/04C08F220/58C08F226/10C08F2/48
CPCA61L24/001A61L24/06C08F261/04C08F2/48A61L2300/622C08F220/585C08F226/10
Inventor 张雪非
Owner SHANGHAI HUIHE HEALTHCARE TECH CO LTD
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