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A kind of nuclear magnetic resonance visualization injectable pH-sensitive self-healing hydrogel and its preparation method and application

A nuclear magnetic resonance and hydrogel technology, which is applied in the fields of chemistry and biomedicine, can solve the problem that the gel cannot be developed, and achieve the effect of reducing the risk of lesions and less trauma.

Inactive Publication Date: 2017-05-03
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to overcome the deficiency that the existing gel cannot be developed, the present invention provides a hydrogel that can be developed by nuclear magnetic resonance, and the gel has the characteristics of being injectable and self-healing within a certain pH range, and its specific technical scheme as follows:

Method used

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  • A kind of nuclear magnetic resonance visualization injectable pH-sensitive self-healing hydrogel and its preparation method and application
  • A kind of nuclear magnetic resonance visualization injectable pH-sensitive self-healing hydrogel and its preparation method and application
  • A kind of nuclear magnetic resonance visualization injectable pH-sensitive self-healing hydrogel and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Preparation of Ch-DTPA

[0044] 1 g of chitosan (Chitosan) was heated to 65° C. with 70 mL of 50 mM dilute hydrochloric acid and stirred for 3 h to dissolve completely. DTPA (0.9102g, 2.3mmol) was dissolved in a small amount of secondary water, and the pH was adjusted to 4.7 with TEMED. NHS (0.3199g, 2.8mmol), EDC (0.5328g, 2.8mmol) were dissolved in 50mM dilute hydrochloric acid solution, mixed with DTPA solution at 0°C and added dropwise to Chitosan solution. Stir the reaction in an oil bath at 75°C for 30h, and continue to stir at room temperature for 12h. After the reaction stopped, put it into a dialysis bag with a molecular weight cut-off of 8k-14k, and use secondary water as the medium for dialysis for 3 days. The dialyzed inner fluid was freeze-dried to obtain Ch-DTPA as light yellow powder. The compound was characterized by FT-IR.

[0045] DTPA, Chitosan, Ch-DTPA and the mixture of DTPA and Chitosan were tested by FT-IR. Depend on figure 1 It can be seen ...

Embodiment 2

[0051] Preparation of Ch-DTPA

[0052] 1 g of chitosan (Chitosan) was heated to 65° C. with 70 mL of 50 mM dilute hydrochloric acid and stirred for 3 h to dissolve completely. DTPA (0.9102g, 2.3mmol) was dissolved in a small amount of secondary water, and the pH was adjusted to 4.7 with TEMED. NHS (0.3199g, 2.8mmol), EDC (0.5328g, 2.8mmol) were dissolved in 50mM dilute hydrochloric acid solution, mixed with DTPA solution at 0°C and added dropwise to Chitosan solution. Stir the reaction in an oil bath at 75°C for 30h, and continue to stir at room temperature for 12h. After the reaction stopped, put it into a dialysis bag with a molecular weight cut-off of 8k-14k, and use secondary water as the medium for dialysis for 3 days. The dialyzed inner fluid was freeze-dried to obtain Ch-DTPA as light yellow powder.

[0053] PEG 1k - Preparation of DF

[0054] Polyethylene glycol PEG 1000 (10.00g, 10.0mmol) was dried overnight in a vacuum oven at 50°C and dissolved in 100mL of dry ...

Embodiment 3

[0058] Preparation of Ch-DTPA

[0059] 1g chitosan Chitosan was heated to 65°C with 70mL 50mM dilute hydrochloric acid and stirred for 3h to dissolve completely. DTPA (1.21 g, 3.1 mmol) was dissolved in a small amount of secondary water, and the pH was adjusted to 4.7 with N,N,N',N'-tetramethylethylenediamine TEMED. N-hydroxysuccinimide NHS (0.43g, 3.72mmol), EDC (0.7131g, 3.72mmol) was dissolved in 50mM dilute hydrochloric acid solution, mixed with DTPA solution at 0°C and added dropwise to Chitosan solution. Stir the reaction in an oil bath at 75°C for 30h, and continue to stir at room temperature for 12h. After the reaction stopped, put it into a dialysis bag with a molecular weight cut-off of 8k-14k, and use secondary water as the medium for dialysis for 3 days. The dialyzed inner fluid was freeze-dried to obtain Ch-DTPA as light yellow powder. The compound was characterized by FT-IR. PEG 4K - Preparation of DA

[0060] Polyethylene glycol PEG 4000, acetic anhydride ...

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Abstract

The invention provides nuclear magnetic resonance visual injectable pH sensitive self-repairing water gel. The gel consists of DTPA-modified chitosan (component A) and polyethylene glycol (component B) of which two ends are subjected to hydroformylation, and the component A solution complexed with Gd<3+> and the component B solution are mixed in a short time at room temperature so as to form in-situ gel. The gel has the pH sensitive self-repairing characteristic, a developing agent is not needed to be repeatedly injected to a patient, and developing can be guaranteed for a long time by using MRI (Magnetic Resonance Imaging), so that the lesion risk caused by Gd<3+> enrichment is reduced. The water gel provided by the invention can serve as drug carriers, embolism or filling materials and tissue scaffold materials in clinical application.

Description

technical field [0001] The invention belongs to the fields of chemistry and biomedicine, and in particular relates to a nuclear magnetic resonance visualized injectable pH-sensitive self-healing hydrogel and its preparation method and application. Background technique [0002] Hydrogel is a polymer cross-linked structure material with water as the dispersion medium. Because it is rich in water, soft and has a certain shape, it usually has excellent biocompatibility and similarity to biological tissues. It has a wide range of applications in the field of biomedicine, and can be used as a drug sustained release matrix material, tissue repair material, etc. Among them, natural polymers such as hyaluronic acid, dextran, alginic acid, chondroitin sulfate, chitosan, pectin, gelatin, fibrin, etc. have the characteristics of excellent biocompatibility, degradability or absorbability , has been deeply studied and widely used in the design and synthesis of medical hydrogels. [0003...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K49/18A61K49/12A61K47/36A61K47/10A61L27/26A61L31/04A61L31/06A61L31/16A61L27/54A61L27/52A61L31/14
Inventor 刘芝兰刘佳吴光耀文之李乐王磊张留杰杜丽娜卓仁禧
Owner WUHAN UNIV
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