AU2021103980A4 - A Preparation Method of Bone Scaffold Composite Material - Google Patents

A Preparation Method of Bone Scaffold Composite Material Download PDF

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Publication number
AU2021103980A4
AU2021103980A4 AU2021103980A AU2021103980A AU2021103980A4 AU 2021103980 A4 AU2021103980 A4 AU 2021103980A4 AU 2021103980 A AU2021103980 A AU 2021103980A AU 2021103980 A AU2021103980 A AU 2021103980A AU 2021103980 A4 AU2021103980 A4 AU 2021103980A4
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Prior art keywords
bone
preparation
fetal bovine
tcp
calcined
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AU2021103980A
Inventor
Xiaopan HU
Kangli Jiao
Zhiqiang Li
Tianzhu Song
Xiaodong Xie
Jumei ZHANG
Xuan Zhang
Xin Zheng
Jianye ZHOU
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Northwest Minzu University
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Northwest Minzu University
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/36Materials for grafts or prostheses or for coating grafts or prostheses containing ingredients of undetermined constitution or reaction products thereof, e.g. transplant tissue, natural bone, extracellular matrix
    • A61L27/3604Materials for grafts or prostheses or for coating grafts or prostheses containing ingredients of undetermined constitution or reaction products thereof, e.g. transplant tissue, natural bone, extracellular matrix characterised by the human or animal origin of the biological material, e.g. hair, fascia, fish scales, silk, shellac, pericardium, pleura, renal tissue, amniotic membrane, parenchymal tissue, fetal tissue, muscle tissue, fat tissue, enamel
    • A61L27/3608Bone, e.g. demineralised bone matrix [DBM], bone powder
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/14Macromolecular materials
    • A61L27/20Polysaccharides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2430/00Materials or treatment for tissue regeneration
    • A61L2430/02Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Public Health (AREA)
  • Biomedical Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Transplantation (AREA)
  • General Health & Medical Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Animal Behavior & Ethology (AREA)
  • Epidemiology (AREA)
  • Dermatology (AREA)
  • Medicinal Chemistry (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Molecular Biology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Botany (AREA)
  • Zoology (AREA)
  • Urology & Nephrology (AREA)
  • Orthopedic Medicine & Surgery (AREA)
  • Materials For Medical Uses (AREA)

Abstract

The invention discloses a preparation method of bone scaffold composite material, which comprises the following steps: 1) Preparation of -TCP calcined bone block; 2) Preparation of j-TCP/Zn2+ calcined bone block; 3) Preparation of -TCP/CS composite scaffold materials; 4) Preparation of j-TCP/Zn2+/CS porous composite scaffolds. The beneficial effects of the invention are as follows: the invention provides a preparation method of bone scaffold composite material. The fetal bovine bone (p-tricalcium phosphate) is prepared by secondary calcination of fetal bovine cancellous bone by ammonium dihydrogen phosphate method and then modified by the double surface of + zinc + chitosan. It is a bone scaffold material with good biocompatibility and strong comprehensive bone repair ability; at the same time, with the large-scale popularization of serum treatment, China's fetal bovine serum manufacturers began to develop on a large scale, the use of fetal bovine serum is gradually increasing, while the natural fetal bovine bone, the remaining material for the production of fetal bovine serum is wasted, the full use of it can reduce the cost of two medical industries.

Description

The invention discloses a preparation method of bone scaffold composite material, which
comprises the following steps: 1) Preparation of -TCP calcined bone block; 2) Preparation of
j-TCP/Zn 2+ calcined bone block; 3) Preparation of -TCP/CS composite scaffold materials; 4)
Preparation of j-TCP/Zn 2+/CS porous composite scaffolds. The beneficial effects of the
invention are as follows: the invention provides a preparation method of bone scaffold
composite material. The fetal bovine bone (p-tricalcium phosphate) is prepared by secondary
calcination of fetal bovine cancellous bone by ammonium dihydrogen phosphate method and
then modified by the double surface of + zinc + chitosan. It is a bone scaffold material with
good biocompatibility and strong comprehensive bone repair ability; at the same time, with the
large-scale popularization of serum treatment, China's fetal bovine serum manufacturers began
to develop on a large scale, the use of fetal bovine serum is gradually increasing, while the
natural fetal bovine bone, the remaining material for the production of fetal bovine serum is
wasted, the full use of it can reduce the cost of two medical industries.
A Preparation Method of Bone Scaffold Composite Material
Technical Field The invention relates to the technical field of medical material preparation, in particular to a
preparation method of bone scaffold composite material.
Background Although the effectiveness and safety of calcined natural bovine cancellous bone have been
recognized, there are still some problems in its application and development. Take Bio-OSS
bone meal from Switzerland as an example. Although it has absolute dominance in the market, it
has the following disadvantages : (1) It is expensive, which not only hinders the popularity of
bone implantation surgery, but also brings economic losses to patients; (2) Powdered osteogenic
materials have poor ability in osteogenic properties and are easy to lead to tissue necrosis; (3)
Only calcination de-immunization process, no surface modification, lack of bone growth
promotion. The brand sales of "GeRui" from Shanxi are not only difficult to shake the dominant
position of imported materials, and that, like "Bio-OSS", it has not been treated with surface
modification and still lacks the promotion effect of bone growth.
Content of invention
The purpose of the invention is to provide a method for preparing bone scaffold composite
material in view of the defects in the existing technology. It innovates and improves the
calcination process of natural fetal bovine bone by using ammonium dihydrogen phosphate
calcination method. At the same time, with the popularization of the large area of serum
treatment, China's fetal bovine serum manufacturers began to develop on a large scale. The
dosage of fetal bovine serum is gradually increasing, and the natural fetal bovine bone, the
remaining material for the production of fetal bovine serum, is wasted. The full use of it can
reduce the cost of the two medical industry.
In order to realize the above purpose, the technical scheme provided by the invention is: a preparation method of bone scaffold composite material, including the following steps:
1) Preparation of -TCP calcined bone block:
The cancellous bone parts of fresh fetal bovine bones were sawn into cuboid bone blocks with
the sizes of 5mmx5mmxlcm and 5mmx5mmx4cm, the bone blocks were boiled with deionized
water to degrease for protein for 4h, then desugared in 0.25mol/L NaOH solution at 90°C for
-30min, and soaked in 10% H202 solution for 10-15min after bleaching, to remove part of the
organic material in cancellous bone.
The above treated bone pieces were soaked out with filter paper, dried at 50°C for 12h, then
calcined in a resistance furnace, slowly raised to 800°C at a heating rate of 5C/min, and then
cooled to room temperature naturally after 6h.
The cuboid bone block calcined at 800°C was cleaned and dried by ultrasonic with the ultrasonic
power of 480W, the cleaning time of 30min, the drying temperature of 50°C and the drying time
of 24h. Then the cuboid bone block was immersed in a 0.5mol/L NH4H2PO4 solution at room
temperature for 24h, and dried at 50°C for Id, then the cuboid bone block was calcined at high
temperature in a resistance furnace for secondary calcination, the calcined p-TCP bone
fragments were obtained by slowly heating up to 1000°C at 10 C/min and holding time for 4h.
2) Preparation of -TCP/Zn 2+ calcined bone block:
The p-TCP/Zn 2 +calcined bone blocks prepared in Step 1) were immersed in 500mL 0.25 mol/L
ZnCl2 solution for 1h at 60 °C, then dried and calcined at 1200°C for1h to prepare p-TCP/Zn2+
calcined bone block containing 0.4%wt zinc.
3) Preparation of The p-TCP/CS composite scaffold
2g chitosan was weighed and sterilized by ultraviolet radiation for 6h. 200mL of 10g/L acetic
acid was added under sterile conditions and fully dissolved under magnetic stirring. It was
stored at 4C for later use ; Under aseptic conditions, the 100gp-TCP calcined bone blocks
obtained from the sterilized steps 1) were placed in a 250mL glass reagent bottle with rubber stopper, and the prepared chitosan solution was added. The chitosan solution entered the porous cavity of the material after negative pressure suction. The solution was placed at 4°C for 24h, then the solution was removed and dried to obtain the composite material; then the composite was soaked in sterile dilute ammonia solution for 12 h, washed with 0.01 mol/L PBS of pH 7.4 to neutral, and dried to prepare p-TCP/CS composite containing 0.7%wt.
4) Preparation of The p-TCP/Zn2+/CS porous composite scaffolds
The p-TCP/Zn2+ calcined bone blocks obtained from the disinfected step 2) were immersed in
CS solution under negative pressure, sucked and washed to neutral as described in step 3, the
p-TCP/Zn2+/CS porous composite scaffold material containing zinc 0.4%wt and CS 0.7%wt
was prepared after drying.
The beneficial effects of the invention are as follows: the invention provides a preparation
method for bone scaffold composite material: the invention provides a preparation method for a
bone scaffold composite material. The fetal bovine bone (p-tricalcium phosphate) is prepared by
secondary calcination of fetal bovine cancellous bone by ammonium dihydrogen phosphate
method and then modified by the double surface of + zinc + chitosan. It is a bone scaffold
material with good biocompatibility and strong comprehensive bone repair ability; at the same
time, with the large-scale popularization of serum treatment, China's fetal bovine serum
manufacturers began to develop on a large scale, the use of fetal bovine serum is gradually
increasing, while the natural fetal bovine bone, the remaining material for the production of fetal
bovine serum is wasted, the full use of it can reduce the cost of two medical industries.
Brief Description of the Drawings
Fig.1 shows the X-ray diffraction analysis of calcined bone.
Wherein, horizontal and vertical coordinates are: diffraction angle 20, diffraction intensity; a:
X-ray diffraction map of adult cow bone calcined at 800°C. The red line is the diffraction broken
line of adult cow bone, and the black line is the diffraction peak map of standard Ca(PO4)(OH); b: X-ray diffraction pattern of fetal bovine bone calcined at 800°C. The red line is the diffraction broken line of fetal bovine bone, and the black line is the diffraction peak pattern of standard
Ca5(PO4)(OH). c: diffusion peak diagram of calcined adult bovine bones by sodium
pyrophosphate method (black) and ammonium dihydrogen phosphate method (red) respectively;
the purple is the diffraction peak of Ca 3 (PO 4 ) 2 , the green is the diffraction peak of Ca(PO 4 )(OH);
d: diffraction peaks of fetal bovine bones calcined by sodium pyrophosphate method (black) and
ammonium dihydrogen phosphate method (red) respectively; the purple is the diffraction peak
of Ca3 (P04)2 standard, and the green is the diffraction peak of Ca(PO4)(OH) standard.
%-ALA'V111
1. A preparation method of bone scaffold composite material is characterized in that it includes
the following steps:
1) Preparation of -TCP calcined bone block:
The cancellous bone parts of fresh fetal bovine bones were sawn into cuboid bone blocks with
the sizes of 5mmx5mmx lcm and 5mmx5mmx4cm, the bone blocks were boiled with deionized
water to degrease for protein for 4h, then desugared in 0.25mol/L NaOH solution at 90°C for
-30min, and soaked in 10% H20 2 solution for 10-15min after bleaching, to remove part of the
organic material in cancellous bone.
The above treated bone pieces were soaked out with filter paper, dried at 50°C for 12h, then
calcined in a resistance furnace, slowly raised to 800°C at a heating rate of 5C/min, and then
cooled to room temperature naturally after 6h.
The cuboid bone block calcined at 800°C was cleaned and dried by ultrasonic with the ultrasonic
power of 480W, the cleaning time of 30min, the drying temperature of 50°C and the drying time
of 24h, then the cuboid bone block was immersed in 0.5mol/L NH 4 H2 PO 4 solution at room
temperature for 24h, and dried at 50°C for Id, then the cuboid bone block was calcined at high
temperature in a resistance furnace for secondary calcination, the calcined p-TCP bone fragments
were obtained by slowly heating up to 1000°C at 10°C/min and holding time for 4h.
2) Preparation of -TCP/Zn 2+calcined bone:
The p-TCP/Zn2+calcined bone blocks prepared in Step 1) were immersed in 500mL 0.25 mol/L
ZnCl2 solution for 1h at 60 °C, then dried and calcined at 1200°C for1h to prepare p-TCP/Zn2+ calcined bone block containing 0.4%wt zinc.
3) Preparation of The p-TCP/CS composite scaffold
2g chitosan was weighed and sterilized by ultraviolet light for 6h and 200mL of10g/L acetic
acid was added under aseptic conditions and fully dissolved under magnetic stirring, then stored
at 4C for later use; under aseptic conditions, the 100gp-TCP calcined bone blocks obtained from
%-L11 I111
the sterilized steps 1) were placed in a 250mL glass reagent bottle with rubber stopper, and the
prepared chitosan solution was added., the chitosan solution entered the porous cavity of the
material after negative pressure suction, the solution was placed at 4C for 24 h, then the solution
was removed and dried to obtain the composite material; then the composite was soaked in
sterile dilute ammonia solution for 12 h, washed with 0.01 mol/L PBS of pH 7.4 to neutral, and
dried to prepare p-TCP/CS composite containing 0.7%wt.
4) Preparation of the p-TCP/Zn 2+/CS porous composite scaffolds
The p-TCP/Zn2+ calcined bone blocks obtained from the disinfected step 2) were immersed in
CS solution under negative pressure, sucked and washed to neutral as described in step 3, the
p-TCP/Zn2+/CS porous composite scaffold material containing zinc 0.4%wt and CS 0.7%wt was
prepared after drying.
DRAWINGS
Adult Bone 800℃ Fetal Bovine Bone 800℃ 2021103980
Adult Bone 1000℃ Fetal Bovine Bone 1000℃
FIG. 1
AU2021103980A 2021-07-08 2021-07-08 A Preparation Method of Bone Scaffold Composite Material Ceased AU2021103980A4 (en)

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Application Number Priority Date Filing Date Title
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AU2021103980A4 true AU2021103980A4 (en) 2021-09-09

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114053482A (en) * 2021-11-22 2022-02-18 江苏苏伯纳生物科技有限公司 Preparation method of bionic artificial bone with natural spatial structure
CN115645620A (en) * 2022-11-13 2023-01-31 江西斯凯复医疗科技有限公司 Preparation method of calcined bone

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114053482A (en) * 2021-11-22 2022-02-18 江苏苏伯纳生物科技有限公司 Preparation method of bionic artificial bone with natural spatial structure
CN115645620A (en) * 2022-11-13 2023-01-31 江西斯凯复医疗科技有限公司 Preparation method of calcined bone
CN115645620B (en) * 2022-11-13 2023-10-24 江西斯凯复医疗科技有限公司 Preparation method of calcined bone

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