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Polymer hollow sphere with PEGylation on surface and preparation method thereof

A polymer and hollow sphere technology, applied in the field of polymer materials, can solve the problems of increasing preparation steps, many steps, and complicated preparation process, and achieve the effects of simple and convenient preparation process, mild reaction conditions, and avoiding harsh conditions

Inactive Publication Date: 2013-12-04
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation method has many steps, the preparation process is complicated, the manufacturing cost is high, and it is easy to cause environmental and energy problems. Moreover, the template material located at the core is removed by chemical corrosion, and it is easy to destroy the PEGylated polymer shell and the hollow polymer contained in the polymer. compound in the ball
[0005] The invention with application number 201010228510.6 discloses a method for preparing microcapsules by layer-by-layer assembly, but the preparation process is cumbersome, and the template material used in the preparation needs to be removed by chemical corrosion to obtain a hollow structure. The strong alkali used Corrosive agents such as strong acid will also cause certain damage to polymer hollow spheres
[0006] The invention with application number 200910030113.5 discloses a method for preparing temperature-sensitive microcapsules. Although the preparation method can avoid the use of templates, it needs to form hollow spheres first, and then use small organic molecules for cross-linking, which increases the preparation steps. The device is relatively complicated, which limits its application prospects, and the introduction of small organic molecules as crosslinking agents often affects the practical application of polymer hollow spheres

Method used

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  • Polymer hollow sphere with PEGylation on surface and preparation method thereof
  • Polymer hollow sphere with PEGylation on surface and preparation method thereof
  • Polymer hollow sphere with PEGylation on surface and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] 500ul of (3-trimethoxysilyl)propyl methacrylate (TMSPMA) and 370ul of polyethylene glycol monomethyl ether methacrylate (PEGMEMA, number average molecular weight Mn=475) were dissolved in 10ml of anhydrous tetrahydrofuran, under nitrogen Stir under the atmosphere to make it fully dissolved, then add 1 mg of azobisisobutyronitrile, stir well, and react at a constant temperature in a 60°C oil bath for 24 hours under a nitrogen atmosphere, then take it out and cool it to room temperature naturally; The product precipitated out, and the precipitate was dried in vacuo to obtain PEGylated polymer P(TMSPMA-co-PEGMEMA).

[0059] The NMR spectrum of the polymer P (TMSPMA-co-PEGMEMA) of gained PEGylation is shown in figure 1 . 4.1ppm as figure 1 The hydrogen peak at the c position shown in the structural formula, 3.9ppm is as figure 1 The hydrogen peak at the d position shown in the structural formula, 3.7ppm is as figure 1 The hydrogen peak at the b position shown in the str...

Embodiment 2

[0080] 500ul of (3-triethoxysilyl)propyl methacrylate (TESPMA) and 370ul of polyethylene glycol methacrylate (PEGMA, number average molecular weight Mn=168) were dissolved in 10ml of anhydrous 1,4-dioxane In the ring, stir it under a nitrogen atmosphere to make it fully dissolve, then add 44mg of azobisisobutyronitrile, stir well, under a nitrogen atmosphere, react at a constant temperature in an oil bath at 90°C for 12 hours, take it out and cool it to room temperature naturally; The resulting reaction product was precipitated by n-hexane, and the precipitate was dried in vacuo to obtain PEGylated polymer P(TESPMA-co-PEGMA). According to NMR calculation, the mass fraction of PTESPMA in the PEGylated polymer was 71%, and the mass fraction of PPEGMA was 29%.

[0081] Gel permeation chromatography showed that the obtained PEGylated polymer P(TMSPMA-co-PEGMA) had a weight average molecular weight of 10000.

[0082] Preparation of Surface PEGylated Polymer Hollow Spheres

[0083...

Embodiment 3

[0087] 500ul of (3-trimethoxysilyl)propyl methacrylate (TMSPMA) and 46ul of polyethylene glycol methacrylate (PEGMA, number average molecular weight Mn=2088) were dissolved in 10ml of anhydrous 1,4-dioxane In the nitrogen atmosphere, stir it to make it fully dissolved, then add 5mg of benzoyl peroxide, stir well, under the nitrogen atmosphere, put it in an oil bath at 80°C, react at constant temperature for 24 hours, take it out and cool it to room temperature naturally; The resulting reaction product was precipitated with alkanes, and the precipitate was dried in vacuo to obtain PEGylated polymer P(TMSPMA-co-PEGMA). The mass fraction of PTMSPMA in P(TMSPMA-co-PEGMA) obtained by NMR calculation is 85%, and the mass fraction of PPEGMA is 15%.

[0088] Gel permeation chromatography showed that the obtained PEGylated polymer P(TMSPMA-co-PEGMA) had a weight average molecular weight of 100,000.

[0089] Preparation of Surface PEGylated Polymer Hollow Spheres

[0090] (1) Dissolve...

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Abstract

The invention discloses a polymer hollow sphere with PEGylation on a surface and a preparation method thereof. The PEGylation polymer is dissolved in organic solvent to formulate PEGylation polymer solution, the PEGylation polymer solution is mixed with water to form emulsion, the emulsion is stirred at a constant temperature of 20 DEG C to 30 DEG C for 24-96 hours, and the polymer hollow sphere with PEGylation on the surface is obtained; and the PEGylation polymer is an irregular polymer with a weight-average molecular weight of 1000-100000 formed by a structural unit shown in formula M1 and the structural unit shown in formula M2, in the irregular polymer, a mass percentage content of the structural unit M1 is 45-99 percent, and the mass percentage content of the structural unit M2 is 1-55 percent. According to the preparation method, the reaction condition is mild, the obtained polymer hollow sphere with PEGylation on the surface is provided with the PEGylation surface, and the polymer hollow sphere is enabled to be more stable through a cross-linked shell structure.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to a polymer hollow sphere with a surface PEGylated and a preparation method thereof. Background technique [0002] Most of the current drug administration methods can only maintain the drug concentration in the human body for a short period of time. The drug concentration in the blood or in vivo tissues fluctuates greatly. When the drug first enters the patient's body, it may exceed the patient's maximum drug tolerance. Dosage, after a period of time, is lower than the effective dose for treating the disease, can not achieve the desired curative effect, and even produces side effects. Frequent small dose administration can adjust the drug concentration in the blood and avoid side effects, but it also brings harm to the patient. Many inconveniences, therefore, it is very necessary to prepare a carrier that can slowly release the drug. Now there are polyhydroxybutyrate, chitosan and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/24C08J3/16C08L33/14C08F220/28C08F2/06C08F2/34C08F2/00
Inventor 杜滨阳陈天有聂晶晶范志强
Owner ZHEJIANG UNIV