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CN-122005955-A - Quick-absorption collagen repair film and preparation method thereof

CN122005955ACN 122005955 ACN122005955 ACN 122005955ACN-122005955-A

Abstract

The application discloses a rapid-absorption collagen repair film and a preparation method thereof, and relates to the technical field of biological materials. The repair membrane is of a double-layer structure and comprises a purified collagen layer and an absorbable polymer spinning layer loaded with inorganic nano particles. The preparation method comprises the steps of purifying animal skin to obtain a purified collagen layer, dispersing and mixing the magnesium yellow feldspar and the hydroxyapatite nano particles respectively, adding the mixed dispersion liquid into an absorbable polymer solution to obtain a composite spinning solution, spinning the composite spinning solution on the surface of the collagen layer by adopting an electrostatic spinning method to form a spinning layer, and drying to obtain the repair film. According to the application, the type, proportion, crystallinity and spatial distribution of inorganic particles are regulated, so that the cooperative enhancement of mechanical properties and biological activity is realized, the repairing film has pH responsive graded release capacity, the degradation behavior can be automatically regulated according to the inflammation intensity, the micro-environment is actively adapted, and the repairing film can be widely applied to the fields of oral soft tissue repairing, tooth Zhou Chuangmian covering and the like.

Inventors

  • GAO HONGYU
  • SHAN YANGANG
  • ZHANG YUFU
  • WANG YULU
  • Cheng Shuimiao
  • ZHANG SHUO
  • YAN SHIZHEN

Assignees

  • 山东博达医疗用品股份有限公司

Dates

Publication Date
20260512
Application Date
20260317

Claims (10)

  1. 1. The preparation method of the rapid absorption collagen repair film is characterized by comprising the following steps of: s1, purifying animal skin, freeze-drying and then uniformly shaving to obtain a purified collagen layer; s2, dispersing the anorthite nano-particles in a solvent to obtain an anorthite pre-dispersion liquid; S3, dispersing the hydroxyapatite nano particles in a solvent to obtain a hydroxyapatite pre-dispersion liquid; S4, mixing the pre-dispersion liquid in the step S2 and the pre-dispersion liquid in the step S3, and carrying out ultrasonic and stirring treatment to obtain a double-particle mixed dispersion liquid; s5, dissolving the absorbable polymer in a solvent to prepare a polymer solution, and then adding the double-particle mixed dispersion liquid obtained in the step S4 into the polymer solution, and uniformly stirring to obtain a composite spinning solution; s6, spinning the composite spinning solution obtained in the step S5 on the surface of the collagen layer by using the purified collagen layer obtained in the step S1 as a receiving substrate and adopting an electrostatic spinning method to form a spinning layer; And S7, drying the double-layer film obtained in the step S6, and removing the solvent to obtain the rapid absorption collagen repair film.
  2. 2. The method according to claim 1, wherein the animal skin in step S1 is mammalian head skin or two skin, and the purification treatment comprises water washing, deashing, softening, hydrogen peroxide soaking, nuclease treatment, buffer washing and freeze drying.
  3. 3. The preparation method according to claim 1, wherein the particle size of the akermanite nano particle in the step S2 is 30-150nm, the solvent is hexafluoroisopropanol, and the pre-dispersion concentration is 0.5-2wt%.
  4. 4. The preparation method according to claim 1, wherein the particle size of the hydroxyapatite nanoparticles in the step S3 is 20-200nm, the solvent is hexafluoroisopropanol, and the pre-dispersion concentration is 0.5-2wt%.
  5. 5. The method according to claim 1, wherein the mass ratio of the hydroxyapatite to the akermanite in the step S4 is 1:1-4:1, the co-ultrasonic treatment power is 150-250W, the time is 10-20 minutes, and the stirring time is 30-60 minutes.
  6. 6. The preparation method of claim 1, wherein the absorbable polymer in the step S5 is one or more of polylactic acid, polyglycolic acid and polylactic acid-glycolic acid copolymer, the concentration of the polymer solution is 5-12wt%, and the total addition amount of the dual inorganic nano particles is 2-15wt% of the mass of the polymer.
  7. 7. The method of claim 1, wherein the drying in step S7 is vacuum drying at a temperature of room temperature to 37 ℃ for 24-72 hours.
  8. 8. The preparation method of claim 1, wherein the nano-particles of the albite in the step S2 are a mixture of albite with three different crystallinity, and the heat treatment conditions of the albite with three crystallinity are respectively 550+/-20 ℃ for 1-2 hours to obtain albite with low crystallinity, 700+/-20 ℃ for 2-3 hours to obtain albite with medium crystallinity, and 850+/-20 ℃ for 3-4 hours to obtain albite with high crystallinity.
  9. 9. The method of claim 1, wherein the repair film is of a spatially partitioned structure and is divided into a central region, an edge region and a transition region, wherein the central region adopts a high-crystallinity melilite dominant formulation, the edge region adopts a low-crystallinity melilite dominant formulation, and the transition region adopts a crystallinity linear gradient transition design.
  10. 10. A rapid-absorption collagen repair film prepared by the method of any one of claims 1-9.

Description

Quick-absorption collagen repair film and preparation method thereof Technical Field The invention relates to a biological material, in particular to a rapid-absorption collagen repair film and a preparation method thereof. Background The quick-absorption collagen repair film is a medical film material which is prepared by taking collagen as a main raw material through a specific process and can be quickly degraded and absorbed in vivo, and is mainly used for short-term healing scenes such as oral soft tissue repair, tooth Zhou Chuangmian coverage, oral ulcer application and the like. It features high biocompatibility, promoting cell adhesion, short degradation period (1-4 weeks generally), and avoiding secondary operation. The currently marketed rapid-absorption collagen membrane is mainly derived from animal connective tissues (such as pigskin and beef achilles tendon) and is prepared by processes of decellularization, purification, freeze-drying and the like. For example: The physical crosslinking method is to increase intermolecular crosslinking of collagen by ultraviolet irradiation, thermal dehydration and other methods, and moderately improve mechanical strength. Chemical cross-linking process includes using glutaraldehyde, carbodiimide (EDC) and other cross-linking agent to form covalent bond between collagen fibers and delay degradation. And the composite modification is to blend collagen with gelatin, chitosan and the like, so as to improve the film forming property and the hydrophilicity. The main technical problems faced by the existing rapid absorption collagen membrane include: the degradation rate does not match the healing cycle-although named "fast absorption" -the actual degradation rate is often difficult to control precisely, some too fast (dissolution in days) leading to loss of barrier function and some too slow (over 4 weeks) possibly triggering foreign body reactions. The mechanical strength is insufficient, the strength of the pure collagen membrane in a wet state is low, the pure collagen membrane is easy to tear, and the pure collagen membrane is difficult to bear the activity of oral muscle and the scouring of saliva. The traditional decellularization process can not completely remove cell components and nucleic acid, and can possibly trigger inflammatory reaction, but delay healing. Disclosure of Invention The embodiment of the application solves the problems in the prior art by providing a rapid-absorption collagen repair film and a preparation method thereof. The embodiment of the application provides a preparation method of a rapid-absorption collagen repair film, which comprises the following steps: s1, purifying animal skin, freeze-drying and then uniformly shaving to obtain a purified collagen layer; s2, dispersing the anorthite nano-particles in a solvent to obtain an anorthite pre-dispersion liquid; S3, dispersing the hydroxyapatite nano particles in a solvent to obtain a hydroxyapatite pre-dispersion liquid; S4, mixing the pre-dispersion liquid in the step S2 and the pre-dispersion liquid in the step S3, and carrying out ultrasonic and stirring treatment to obtain a double-particle mixed dispersion liquid; s5, dissolving the absorbable polymer in a solvent to prepare a polymer solution, and then adding the double-particle mixed dispersion liquid obtained in the step S4 into the polymer solution, and uniformly stirring to obtain a composite spinning solution; s6, spinning the composite spinning solution obtained in the step S5 on the surface of the collagen layer by using the purified collagen layer obtained in the step S1 as a receiving substrate and adopting an electrostatic spinning method to form a spinning layer; And S7, drying the double-layer film obtained in the step S6, and removing the solvent to obtain the rapid absorption collagen repair film. Further, in the step S1, the animal skin is mammalian head skin or two skin layers, and the purification treatment includes water washing, deashing, softening, hydrogen peroxide soaking, nuclease treatment, buffer washing and freeze drying. Further, in the step S2, the particle size of the akermanite nano particles is 30-150nm, the solvent is hexafluoroisopropanol, and the concentration of the pre-dispersion liquid is 0.5-2wt%. Further, in the step S3, the particle size of the hydroxyapatite nano particles is 20-200nm, the solvent is hexafluoroisopropanol, and the concentration of the pre-dispersion liquid is 0.5-2wt%. Further, in the step S4, the mass ratio of the hydroxyapatite to the akermanite is 1:1-4:1, the total ultrasonic treatment power is 150-250W, the time is 10-20 minutes, and the stirring time is 30-60 minutes. Further, the absorbable polymer in the step S5 is one or more of polylactic acid, polyglycolic acid and polylactic acid-glycolic acid copolymer, the concentration of the polymer solution is 5-12wt%, and the total addition amount of the dual inorganic nano particles accounts for 2-15wt% of the mass of