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Injectable hydrogel with high mechanical strength and stability, and preparation method and application thereof

A technology of mechanical strength and stability, applied in the field of biomedical materials, can solve the problems of decreased mechanical properties, poor mechanical strength of injectable hydrogels, etc., to achieve excellent mechanical properties, good biocompatibility, and good long-term stability. Effect

Inactive Publication Date: 2020-06-02
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims to solve the technical problem that the existing injectable hydrogels have poor mechanical strength, and the mechanical properties decrease rapidly due to swelling and degradation under physiological environment, and provide an injectable hydrogel with high mechanical strength and stability. Gel and its preparation method and application

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  • Injectable hydrogel with high mechanical strength and stability, and preparation method and application thereof
  • Injectable hydrogel with high mechanical strength and stability, and preparation method and application thereof
  • Injectable hydrogel with high mechanical strength and stability, and preparation method and application thereof

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Embodiment 1

[0050] Refer to the patent No. 201810670921.7 for the synthesis of hydroxylamino-terminated polyethylene glycol block polymers. The synthesis steps are as follows:

[0051] 1.1 Add 1.5g of guanidine carbonate and 20mL of absolute ethanol to the flask, then add 2.2mL of α-acetyl-γ-butyrolactone and 5.5mL of triethylamine. The reaction was stirred and refluxed at 90° C. for 2 h, and then lowered to room temperature for more than 4 h. The white precipitate was collected, washed 2-3 times with ice ethanol (4° C.), and dried to obtain the first intermediate.

[0052]1.2 Add 1 g of the first intermediate to the flask, then add 20 mL of 1,6-hexamethylene diisocyanate and 1 mL of pyridine. Under the protection of nitrogen, the temperature was raised to 90° C. for 3 h until the solution became completely transparent. Then, the reaction liquid was directly precipitated in 400 mL of n-pentane, and the second intermediate was collected.

[0053] 1.3 Add 0.81 g of N, N'-carbonyldiimidaz...

Embodiment 2

[0060] Synthetic steps of four-arm polyethylene glycol terminated by aldehyde group

[0061] Add 1 g of four-armed polyethylene glycol (molecular weight: 2000 Da), 0.6 g of p-carboxybenzaldehyde, 0.82 g of dicyclohexylcarbodiimide, 0.2 g of 4-dimethylaminopyridine, and 30 mL of tetrahydrofuran into the flask. Under nitrogen condition, react at 40°C for 36h. Afterwards, the reaction solution was filtered, spin-dried and then dissolved in CH 2 Cl 2 in, with 95% CH 2 Cl 2 / 5% MeOH was used as eluent, and the aldylated four-arm PEG2k was separated by silica gel chromatography. The aldehyde-terminated four-armed polyethylene glycol with the structure of formula ii is finally obtained. Such as figure 1 As shown, the nuclear magnetic spectrum proved the successful synthesis of the product. Its aldehyde group capping ratio is 98%, and the number average molecular weight is 2428-2628Da.

Embodiment 3

[0063] Preparation of hydrogel

[0064] The polyethylene glycol block polymer terminated by the hydroxyl amino group with the structure of formula i was dissolved in phosphate buffer (0.0125M, pH=5.2), and prepared into solutions with concentrations of 11.1w / v% and 13.3w / v% respectively , is the first mixed solution. Heat the solution in a water bath at 70°C for 15-20 minutes until the polymer is completely dissolved and a uniform transparent liquid is formed.

[0065] The four-armed polyethylene glycol terminated with aldehyde group having the structure of formula ii was dissolved in phosphate buffer (0.0125M, pH=5.2), and prepared into solutions with concentrations of 6.8w / v% and 8.2w / v%, respectively, as Second mixture.

[0066] Fully mix 750 μL of the 11.1w / v% first mixed solution and 250 μL of the 6.8w / v% second mixed solution at 37°C, and let it stand at 37°C for more than 12 hours to ensure complete gelation and obtain a solute concentration of 10w / v %.

[0067] Ful...

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Abstract

The invention relates to an injectable hydrogel with high mechanical strength and stability, and a preparation method and an application thereof, and belongs to the field of biomedical materials. Thetechnical problems that existing injectable hydrogel is poor in mechanical strength, and the mechanical property is rapidly reduced due to swelling and degradation in a physiological environment are solved. The injectable hydrogel comprises two components, namely a buffer solution dissolved with a hydroxyamino-terminated polyethylene glycol block polymer and a buffer solution dissolved with aldehyde-terminated four-arm polyethylene glycol. The preparation method comprises the following steps: uniformly mixing the two components according to the molar ratio of hydroxyamino to aldehyde of 1: 1,and standing to ensure that the two components are completely gelatinized. The injectable hydrogel can be quickly cured within 20 s, the compression strength can reach 30-40 MPa, and the injectable hydrogel has very good fatigue resistance and mechanical property long-term stability (complete degradation after soaking for 32-44 weeks). The injectable hydrogel is good in biocompatibility, can be applied to the field of biological materials, and particularly has a very good application prospect in the fields of tissue engineering and drug sustained release.

Description

technical field [0001] The invention belongs to the field of biomedical materials, and in particular relates to an injectable hydrogel with high mechanical strength and stability in a physiological environment, a preparation method and application thereof. Background technique [0002] Hydrogel is generally a kind of polymer material composed of three-dimensional cross-linked polymer network and dispersion medium water. Injectable hydrogel is a hydrogel material that can be injected in vitro and gelled in vivo. It has the advantages of minimally invasive transplantation, filling irregular wounds, and carrying cells, drugs, and bioactive molecules. It has received extensive attention in tissue repair and drug carriers. However, limited by the preparation conditions, the mechanical properties of injectable hydrogels are often poor, and they are prone to swelling and degradation in physiological environments, which will not only damage the surrounding tissues but also reduce t...

Claims

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Application Information

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IPC IPC(8): C08J3/075C08L87/00C08L71/02A61L27/26A61L27/50A61L27/52A61K9/06A61K47/34
CPCA61K9/0019A61K9/06A61K47/34A61L27/26A61L27/50A61L27/52A61L2400/06C08J3/075C08J2371/02C08J2387/00C08L71/02C08L87/00
Inventor 杨小牛秦泽昭吕红英俞晓峰袁黎光吴海洋
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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