CN113769159A - Anhydrous calcium phosphate bone cement and preparation method thereof - Google Patents

Anhydrous calcium phosphate bone cement and preparation method thereof Download PDF

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CN113769159A
CN113769159A CN202110965388.9A CN202110965388A CN113769159A CN 113769159 A CN113769159 A CN 113769159A CN 202110965388 A CN202110965388 A CN 202110965388A CN 113769159 A CN113769159 A CN 113769159A
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parts
powder
solid
suspending agent
liquid
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车七石
单玲星
赵澎
张俊辉
刘少辉
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Guangzhou Rainhome Pharm and Tech Co Ltd
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Guangzhou Rainhome Pharm and Tech Co Ltd
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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
    • A61L27/02Inorganic materials
    • A61L27/12Phosphorus-containing materials, e.g. apatite
    • 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
    • A61L27/18Macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • 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
    • A61L2400/00Materials characterised by their function or physical properties
    • A61L2400/06Flowable or injectable implant compositions
    • 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)
  • Chemical & Material Sciences (AREA)
  • Transplantation (AREA)
  • Dermatology (AREA)
  • Medicinal Chemistry (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Epidemiology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials For Medical Uses (AREA)

Abstract

The invention discloses anhydrous calcium phosphate cement, which is characterized by comprising mixed solid-phase powder and liquid-phase components; the solid-phase powder comprises the following components in parts by mass: 60-80 parts of calcium phosphate powder and 10-30 parts of a suspending agent, wherein the suspending agent comprises guar gum, konjac glucomannan and artemisia glue; the liquid phase component comprises the following components in parts by mass: 30-60 parts of a solvent. The bone cement prepared by the invention is simple to operate, the sample is placed in the container and injected or filled when in use, and the solid phase and the liquid phase do not need to be mixed on site, so that the operation time and the pollution risk are reduced. The added suspending agent and solvent can lead the bone cement to be sealed and stored in a container, has good fluidity and injection performance, does not separate solid from liquid, is stable paste in the container, is gradually solidified by the liquid in the environment after being filled into the bone defect part, and greatly shortens the solidification time.

Description

Anhydrous calcium phosphate bone cement and preparation method thereof
Technical Field
The invention belongs to the field of medical materials, relates to bone cement, and particularly relates to anhydrous calcium phosphate bone cement and a preparation method thereof.
Background
The calcium phosphate cement is an orthopedic material and can be self-solidified under physiological condition to obtain solidified product similar to human bone tissue. The calcium phosphate bone cement has good biocompatibility and can be arbitrarily shaped according to the defect part. After being hydrated, the calcium phosphate cement is converted into hydroxyapatite which can guide bone growth. In general, the use of injectable calcium phosphate cement requires a doctor to blend a solid phase with a liquid phase on site, which not only prolongs the operation time, but also easily causes uneven mixing, risks of contamination, and fails to ensure the repeatability of the operation effect.
Patent CN201710378895.6 discloses a calcium phosphate cement containing konjac glucomannan and a preparation method and application thereof, the konjac glucomannan forms hydrogen bonds among molecules in an aqueous solution to promote KGM partial crystallization, and the aqueous solution state is converted to a gel state to form a gel with a three-dimensional structure. KGM has large molecular weight, no charge, strong hydration capability and excellent thickening performance. However, only the thickening effect of konjac glucomannan in aqueous calcium phosphate cement is disclosed.
US Patent 6793725(2004) discloses that glycerin, polypropylene glycol and low molecular weight liquid PEG can be used as non-aqueous phase solidifying liquid to prepare injectable calcium phosphate cement in an anhydrous state, and solid-liquid phases are mixed in advance, so that the blending time of doctors during surgery can be reduced. However, the anhydrous bone cement is liable to be delaminated and precipitated, which affects injectability and self-setting property of the bone cement, and the anhydrous bone cement does not contain water, and thus, when it enters a bone defect, the outer portion of the bone cement comes into contact with body fluid, while the inner portion does not contain water, so that the inner setting speed is slower than that of the outer portion, which deteriorates mechanical properties of the bone cement after it is set.
Therefore, there is a need for an anhydrous bone cement which can maintain coexistence of solid and liquid, does not cause delamination and precipitation, and does not affect injectability of the bone cement and self-setting performance after injection.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the anhydrous calcium phosphate bone cement, which can keep coexistence of solid and liquid, does not generate layering and precipitation, and does not influence the injectability of the bone cement and the self-solidifying performance after injection.
In order to achieve the purpose, the invention adopts the technical scheme that:
an anhydrous calcium phosphate cement, which is characterized by comprising solid-phase powder and liquid-phase components; the solid-phase powder comprises the following components in parts by mass: 60-80 parts of calcium phosphate powder and 10-30 parts of a suspending agent, wherein the suspending agent comprises guar gum, konjac glucomannan and artemisia glue; the liquid phase component comprises the following components in parts by mass: 30-60 parts of a solvent;
preferably, the solid-phase powder comprises the following components in parts by mass: 60-70 parts of calcium phosphate powder and 10-20 parts of a suspending agent, wherein the suspending agent comprises guar gum, konjac glucomannan and artemisia glue; the liquid phase component comprises the following components in parts by mass: 30-40 parts of a solvent.
Cationic guar gum is a water-soluble high molecular polymer with the chemical name of guar gum hydroxypropyl trimethyl ammonium chloride. The natural guar gum is used as a raw material, the endosperm part left after the epidermis and the embryo are removed mainly contains galactose and mannose, the natural guar gum is dried, crushed, pressurized, hydrolyzed, precipitated by ethanol solution, centrifugally separated, dried and reacted with water-loss condensed glycerol ether trimethyl ammonium chloride to prepare the guar gum.
Artemisia desertorum glue: artemisia glue Sa-son seed gum is also called Artemisia seed glue. The artemisia glue is mainly composed of glucose, galactose, mannose, arabinose, xylose and the like, is a polysaccharide substance with a cross-linked structure, and has high viscosity (1% aqueous solution reaches 9000 Pa.s) which is 1800 times of that of gelatin. Is insoluble in water but can be uniformly dispersed in water, and can be swelled into egg white-like colloid after absorbing water for tens of times.
Konjac glucomannan: the natural high-molecular soluble dietary fiber is also called KGM, is a good product of all dietary fibers, has high water retention, expansibility, thickening property, gel property, emulsifying property, suspension property, cohesiveness and the like, has better performance than common food gums such as agar, carrageenan, gelatin and the like, and is increasingly widely applied as a food additive.
Guar gum, artemisia desertorum gum and konjac glucomannan can be used as thickening agents in aqueous solution, however, the guar gum and the konjac glucomannan are soluble in water and insoluble in glycerol, the artemisia desertorum gum is insoluble in water and is in a limited water absorption swelling state in water, the gum powder is added into the water to be stirred, most of the gum powder is aggregated into lumps and can not be well dispersed.
Compared with calcium phosphate cement containing aqueous solution, the anhydrous calcium phosphate cement needs to have stable suspension property, no solid-liquid separation, no hydration of the solid in an anhydrous state, good injection property and stable preservation at normal temperature.
Preferably, the mass ratio of guar gum, konjac glucomannan and artemisia glue in the suspending agent is 2-4: 3-5: 3-5, preferably, the mass ratio of the guar gum, the konjac glucomannan and the artemisia desertorum gum as the suspending agent is 2-3: 3-4: 3-4; preferably, the mass ratio of guar gum, konjac glucomannan and artemisia glue in the suspending agent is as follows: 3:4: 4;
preferably, the mass ratio of the solid-phase powder to the liquid phase is 1 (0.2-0.6).
Preferably, the calcium phosphate in the solid phase powder is selected from one or more of tricalcium phosphate, tetracalcium phosphate, octacalcium phosphate, anhydrous calcium hydrophosphate, calcium hydrophosphate dihydrate, calcium biphosphate, calcium pyrophosphate, hydroxyapatite, fluorapatite, strontium apatite and carbonate-containing apatite.
Preferably, in the liquid phase component, the solvent is one or more of glycerol, polyethylene glycol or dimethyl silicone oil.
Preferably, the solid phase powder comprises the following components in parts by mass: 70 parts of calcium phosphate powder and 20 parts of suspending agent; the calcium phosphate powder is alpha-tricalcium phosphate with particle size of 10-200 μm; the suspending agent comprises guar gum, konjac glucomannan and artemisia glue; the mass ratio of guar gum, konjac glucomannan and artemisia glue in the suspending agent is 2-4: 3-5: 3-5; the liquid phase component comprises the following components in parts by mass: 45 parts of solvent, wherein the solvent in the liquid phase component is glycerol, and the preparation method of the artemisia glue comprises the following steps: dissolving commercially available Artemisia desertorum gum powder in deionized water according to the ratio of 1:4-8 to prepare colloid, and grinding for 2-4h after vacuum freeze drying to obtain Artemisia desertorum gum powder.
The invention also provides a preparation method of the bone cement, which comprises the steps of uniformly mixing the calcium phosphate and the suspending agent to prepare solid-phase powder, adding the liquid-phase component in proportion to prepare paste, and hermetically storing the paste sample in a container at 4-50 ℃.
The bone cement can be stored at normal temperature, is convenient to store, does not need to be prepared into paste in advance, can be injected or filled, does not need to mix a solid phase and a liquid phase when being used by a doctor, shortens the operation time, and reduces the pollution risk in the operation process. The paste does not contain water, can not be hydrated, has the storage time of more than 1 year, is beneficial to the commercial popularization and application of the product, and generates a curing reaction with water after being filled into a bone defect part to generate hydroxyapatite.
The invention also provides the application of the anhydrous calcium phosphate cement, and the anhydrous calcium phosphate cement is directly injected and filled in a filling mode or by adopting an injector.
The invention has the beneficial effects that:
the anhydrous bone cement prepared by the invention is simple to operate, the sample is placed in the container and injected or filled when in use, and the solid phase and the liquid phase do not need to be mixed on site, so that the operation time and the risk of introducing bacteria are reduced. The added suspending agent and solvent can lead the bone cement to be sealed and stored in a container, has good fluidity and injection performance, does not separate solid from liquid, is stable paste in the container, is gradually solidified by the liquid in the environment after being filled into the bone defect part, and greatly shortens the solidification time.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
The Artemisia glue powder is white amorphous powder, has total sugar content of 90.6%, uronic acid content of 15.8%, and weight average molecular weight of 7.348 × 104The supplier shanghai dingfen chemical technology ltd, cas: 012111-13-2;
konjac glucomannan, cas: 37220-17-0, brand ruibiio;
guar gum, cas: 9000-30-0, supplier: shanxi Chengming Biotech Co., Ltd;
the preparation method of the artemisia glue comprises the following steps: dissolving 10g of commercial artemisia glue powder in 40-80g of deionized water to prepare a glue, and grinding for 2h after vacuum freeze drying to obtain the artemisia glue powder.
Example 1
In one embodiment of the calcium phosphate cement of the present invention, the cement comprises a solid-phase powder and a liquid-phase component;
the solid-phase powder comprises the following components in parts by mass: 60 parts of calcium phosphate powder and 10 parts of suspending agent; the calcium phosphate powder is alpha-tricalcium phosphate with the particle size of 10-200 mu m; the suspending agent comprises guar gum, konjac glucomannan and artemisia glue; the mass ratio of the suspending agent guar gum, the konjac glucomannan and the artemisia glue is 2:3: 3.
the liquid phase component comprises the following components in parts by mass: 30 parts of a solvent; the solvent is glycerol.
The preparation method of the bone cement comprises the steps of preparing calcium phosphate and a suspending agent into solid-phase powder, adding the solid-phase powder into a liquid-phase component according to a proportion, and blending into paste.
Example 2
In one embodiment of the calcium phosphate cement of the present invention, the cement comprises a solid-phase powder and a liquid-phase component;
the solid-phase powder comprises the following components in parts by mass: 70 parts of calcium phosphate powder and 20 parts of suspending agent; the calcium phosphate powder is alpha-tricalcium phosphate with the particle size of 10-200 mu m; the suspending agent comprises guar gum, konjac glucomannan and artemisia glue; the mass ratio of the suspending agent guar gum, the konjac glucomannan and the artemisia glue is 2:3: 3.
the liquid phase component comprises the following components in parts by mass: 40 parts of a solvent; the solvent is glycerol.
The preparation method of the bone cement comprises the steps of preparing calcium phosphate and a suspending agent into solid-phase powder, adding the solid-phase powder into a liquid-phase component according to a proportion, and blending into paste.
Example 3
In one embodiment of the calcium phosphate cement of the present invention, the cement comprises a solid-phase powder and a liquid-phase component;
the solid-phase powder comprises the following components in parts by mass: 80 parts of calcium phosphate powder and 30 parts of suspending agent; the calcium phosphate powder is alpha-tricalcium phosphate with the particle size of 10-200 mu m; the suspending agent comprises guar gum, konjac glucomannan and artemisia glue; the mass ratio of the suspending agent guar gum, the konjac glucomannan and the artemisia glue is 2:3: 3.
the liquid phase component comprises the following components in parts by mass: 60 parts of a solvent; the solvent is glycerol.
The preparation method of the bone cement comprises the steps of preparing calcium phosphate and a suspending agent into solid-phase powder, adding the solid-phase powder into a liquid-phase component according to a proportion, and blending into paste.
Example 4
In one embodiment of the calcium phosphate cement of the present invention, the cement comprises a solid-phase powder and a liquid-phase component;
the solid-phase powder comprises the following components in parts by mass: 70 parts of calcium phosphate powder and 20 parts of suspending agent; the calcium phosphate powder is alpha-tricalcium phosphate with the particle size of 10-200 mu m; the suspending agent comprises guar gum, konjac glucomannan and artemisia glue; the mass ratio of the suspending agent guar gum, the konjac glucomannan and the artemisia glue is 3:4: 4.
The liquid phase component comprises the following components in parts by mass: 40 parts of a solvent; the solvent is glycerol.
The preparation method of the bone cement comprises the steps of preparing calcium phosphate and a suspending agent into solid-phase powder, adding the solid-phase powder into a liquid-phase component according to a proportion, and blending into paste.
Example 5
In one embodiment of the calcium phosphate cement of the present invention, the cement comprises a solid-phase powder and a liquid-phase component;
the solid-phase powder comprises the following components in parts by mass: 70 parts of calcium phosphate powder and 20 parts of suspending agent; the calcium phosphate powder is alpha-tricalcium phosphate with the particle size of 10-200 mu m; the suspending agent comprises guar gum, konjac glucomannan and artemisia glue; the mass ratio of the suspending agent guar gum, the konjac glucomannan and the artemisia glue is 4:5: 5.
The liquid phase component comprises the following components in parts by mass: 40 parts of a solvent; the solvent is glycerol.
The preparation method of the bone cement comprises the steps of preparing calcium phosphate and a suspending agent into solid-phase powder, adding the solid-phase powder into a liquid-phase component according to a proportion, and blending into paste.
Comparative example 1
The comparative example is approximately the same as the example 2, except that the mass ratio of the konjac glucomannan to the artemisia glue in the comparative example 1 is as follows: 5: 3;
comparative example 2
The comparative example is approximately the same as the example 2, except that the mass ratio of the guar gum to the artemisia desertorum gum in the comparative example 2 is as follows: 5: 3;
comparative example 3
The comparative example is approximately the same as the example 2, except that the mass ratio of the guar gum to the konjac glucomannan in the comparative example 3 is as follows: 2: 5;
comparative example 4
This comparative example is the same as example 2 except that comparative example 4 contains no suspending agent.
Comparative example 5
The comparative example is substantially the same as example 2 except that the comparative example 5 comprises guar gum, konjac glucomannan and xanthan gum in the following mass ratio: 2:3: 3;
comparative example 6
This comparative example is the same as example 2 except that in comparative example 6 commercial artemisia glue was used instead of the artemisia glue prepared according to the present invention.
The following performance tests were performed on the anhydrous calcium phosphate cements prepared in examples 1 to 5 and comparative examples 1 to 6.
1. Fluidity of the resin
According to the 7.2 test in the national standards of medicine and pharmacy YY0717-2009, a graduated syringe was used to deliver 0.05ml of bone cement, which was placed in the center of a glass plate, and 180s after tempering, a second glass plate was placed in the center of the top of the bone cement, followed by a heavy piece to give a total weight of 120 g. The weight was removed in 10min and the maximum and minimum diameter of the bone cement was measured.
The results are shown in Table 1, the products of examples 1-5 have good flowability, the maximum diameter of the disks of the flowability test tests of the samples of examples 1-5 is 26mm, the minimum diameter is 24mm, the flowability can be significantly improved by adding the suspending agent, the specification of iso6876 is met, and the diameter of the samples is more than 20 mm. The bone cement can reach the tip of the root canal, so that when the anhydrous calcium phosphate bone cement of examples 1 to 5 is used for filling the tooth, the gutta percha tip is not needed, and the foreign body stimulation caused by the fact that the gutta percha tip root filling material exceeds the root tip can be avoided.
2. Curing time
The bone cements of examples 1 to 5 and comparative examples 1 to 6 were filled into small paper rings having a diameter of 8mm and a height of 12mm, and both ends of the paper rings were closed with plastic films. In each example, 3 samples are prepared, 30 samples are counted, the prepared samples are immersed in a culture dish filled with SBF solution, the culture dish is placed in a constant temperature and humidity box with 37 ℃ and 100% humidity, the SBF solution can permeate into bone cement through paper sheets, the setting time is measured by a Vicat instrument, during measurement, a Vicat needle is in contact with the surface of the cement, screws are tightened, the cement is suddenly loosened within 1s-2s, the Vicat needle vertically and freely sinks into cement paste, the sinking distance of each time is recorded, the operation is repeated once every 0.1h, and when the sinking of the needle body into the cement paste is not more than 1mm, the initial setting time is set.
3. Measurement of collapse resistance
And (3) injecting 1g of anhydrous calcium phosphate cement into a beaker filled with 30mL of SBF solution through an injector, shaking for 1h in a constant-temperature shaking table at 60rpm and 37 ℃, and calculating the collapsibility of the anhydrous calcium phosphate cement. The collapsibility is the percentage of the mass remaining after the calcium phosphate cement slurry was cured in SBF to the total mass of calcium phosphate cement before curing, and the results are shown in table 1.
TABLE 1
Figure DEST_PATH_IMAGE002
The bone cements of examples 1-5 have better fluidity, which indicates that the addition of the suspending agent can improve the fluidity and thus the injection performance of the bone cement, and the setting time of examples 1-5 is shorter than that of comparative examples 1-6, which indicates that different ratios of the suspending agent affect the setting time of the bone cement. The collapsibility of examples 1 to 5 was lower than that of comparative examples 1 to 6, and the suspending agent could improve the collapsibility resistance of the bone cement.
4. Compressive strength
The bone cements of examples 1 to 5 and comparative examples 1 to 6 were filled into small paper rings of 5mm diameter and 8mm height, and both ends of the paper rings were closed with plastic films. The bone cement was put into a petri dish containing an SBF solution, the petri dish was put into a constant temperature and humidity chamber with a humidity of 100%, the bone cement was taken out after 3 days of immersion, the compressive strength was measured with a universal material testing machine, and the loading rate was 1mm/min, and the results are shown in table 2.
5. Flexural Strength
Tested according to appendix C of the Chinese people's republic of China medical industry Standard YY 0271.2-2016.
The method comprises the following steps:
the cement is filled into a mould in c.2.1 during the working time of the cement, after curing, the sample is removed from the mould, after storage in water at 37 ℃ for 24h, the samples of examples 1-5 and comparative examples 1-5 are removed from the water bath, the test is transferred to a flexural strength test apparatus operating according to the procedure C3, the sample is placed in the centre of the test fixture perpendicular to the three cylinders, the sample is removed from the water bath within 10s, the sample is loaded at a crosshead speed of 0.75mm/min until breaking and the maximum load applied to the sample is recorded.
The flexural strength, σ, was calculated as follows: MPa;
σ=3FL/2bh2
in the formula:
f-maximum load applied to the specimen in cattle (N);
l-distance between two supporting points, unit is millimeter (mm), and accurate to 0.01 mm;
b-the width in millimeters of the middle of the sample measured before testing;
h-height in millimeters measured in the middle of the specimen before testing.
The results are shown in Table 2.
TABLE 2
Group of Dissolution rate (%) Compressive strength (MPa) Flexural Strength (MPa)
Example 1 2.1 26.3 10.6
Example 2 1.2 33.4 13.2
Example 3 1.9 28.6 9.4
Example 4 1.6 31.2 11.3
Example 5 1.7 32.4 12.4
Comparative example 1 3.1 19.2 6.5
Comparative example 2 3.2 18.6 7.6
Comparative example 3 4.2 18.3 6.3
Comparative example 4 6.8 13.9 5.1
Comparative example 5 5.2 15.9 5.9
Comparative example 6 5.3 17.9 5.6
The compression strength and the flexural strength of the examples 1 to 5 are higher than those of the comparative examples 1 to 6, which shows that the addition of the suspending agent can enhance the mechanical properties of the bone cement, not only improve the compression strength of the bone cement, but also improve the flexural strength, expand the application range of the bone cement, can be used for filling tooth roots and avoid the fracture of the bone cement.
6. Storage time:
the samples of examples 1 to 5 and comparative examples 1 to 5 were placed in a sealed container and stored at room temperature for 30 days, 2 months, 6 months, and 12 months, and the phases of the samples were observed. The products of examples 1-5 can be stored for 12 months, the product performance is the same as that of the product just prepared, and the products of comparative examples 1-5 can cause solid-liquid separation when being placed for more than 2 months.
TABLE 2 product Performance test results
Group of 30 days 2 month 6 month 12 month
Example 1 The product is not solidified and solid-liquid is not separated The product is not solidified and solid-liquid is not separated The product is not solidified and solid-liquid is not separated The product is not solidified and solid-liquid is not separated
Example 2 The product is not solidified and solid-liquid is not separated The product is not solidified and solid-liquid is not separated The product is not solidified and solid-liquid is not separated The product is not solidified and solid-liquid is not separated
Example 3 The product is not solidified and solid-liquid is not separated The product is not solidified and solid-liquid is not separated The product is not solidified and solid-liquid is not separated The product is not solidified and solid-liquid is not separated
Example 4 The product is not solidified and solid-liquid is not separated The product is not solidified and solid-liquid is not separated The product is not solidified and solid-liquid is not separated The product is not solidified and solid-liquid is not separated
Example 5 The product is not solidified and solid-liquid is not separated The product is not solidified and solid-liquid is not separated The product is not solidified and solid-liquid is not separated The product is not solidified and solid-liquid is not separated
Comparative example 1 The product is not solidified and solid-liquid is not separated The product is not solidified and is separated from solid and liquid The product is not solidified and is separated from solid and liquid The product is not solidified and is separated from solid and liquid
Comparative example 2 The product is not solidified and solid-liquid is not separated The product is not solidified and is separated from solid and liquid The product is not solidified and is separated from solid and liquid The product is not solidified and is separated from solid and liquid
Comparative example 3 The product is not solidified and solid-liquid is not separated The product is not solidified and is separated from solid and liquid The product is not solidified and is separated from solid and liquid The product is not solidified and is separated from solid and liquid
Comparative example 4 The product is not solidified and is separated from solid and liquid The product is not solidified and is separated from solid and liquid The product is not solidified and is separated from solid and liquid The product is not solidified and is separated from solid and liquid
Comparative example 5 The product is not solidified and solid-liquid is not separated The product is not solidified and is separated from solid and liquid The product is not solidified and is separated from solid and liquid The product is not solidified and is separated from solid and liquid
In conclusion, the bone cement prepared by the invention is simple to operate, the added suspending agent can enable the bone cement to be hermetically stored in a container, the bone cement has good fluidity and injection performance, solid and liquid are not separated, the bone cement is stable paste in the container and is gradually solidified by liquid in the environment after being filled into a bone defect part, and the solidification time is greatly shortened.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (10)

1. An anhydrous calcium phosphate cement, characterized by comprising a solid phase powder and a liquid phase component mixed; the solid-phase powder comprises the following components in parts by mass: 60-80 parts of calcium phosphate powder and 10-30 parts of a suspending agent, wherein the suspending agent comprises guar gum, konjac glucomannan and artemisia glue; the liquid phase component comprises the following components in parts by mass: 30-60 parts of a solvent; preferably, the solid-phase powder comprises the following components in parts by mass: 60-70 parts of calcium phosphate powder and 10-20 parts of a suspending agent, wherein the suspending agent comprises guar gum, konjac glucomannan and artemisia glue; the liquid phase component comprises the following components in parts by mass: 30-40 parts of a solvent.
2. The bone cement of claim 1, wherein the suspending agent comprises guar gum, konjac glucomannan and artemisia glue in a mass ratio of 2-4: 3-5: 3-5, preferably, the mass ratio of the guar gum, the konjac glucomannan and the artemisia desertorum gum as the suspending agent is 2-3: 3-4: 3-4.
3. The bone cement of claim 1, wherein the suspending agent comprises guar gum, konjac glucomannan and artemisia glue in a mass ratio of: 3:4:4.
4. The bone cement of claim 1, wherein the mass ratio of the solid phase powder to the liquid phase is 1 (0.2-0.6).
5. The bone cement of claim 1, wherein the artemisia glue is prepared by the following method: dissolving commercially available Artemisia desertorum gum powder in deionized water according to the ratio of 1:4-8 to prepare colloid, and grinding for 2-4h after vacuum freeze drying to obtain Artemisia desertorum gum powder.
6. A bone cement according to claim 1, wherein the calcium phosphate in the solid phase powder is selected from one or more of tricalcium phosphate, tetracalcium phosphate, octacalcium phosphate, anhydrous calcium hydrogen phosphate, calcium hydrogen phosphate dihydrate, calcium dihydrogen phosphate, calcium pyrophosphate, hydroxyapatite, fluorapatite, strontium apatite, and carbonate-containing apatite.
7. The bone cement of claim 1, wherein the solvent in the liquid phase component is one or more of glycerol, polyethylene glycol 600, or dimethyl silicone oil.
8. A bone cement as claimed in any one of claims 1 to 7, wherein the solid phase powder comprises the following components in parts by mass: 70 parts of calcium phosphate powder and 20 parts of suspending agent; the calcium phosphate powder is alpha-tricalcium phosphate with particle size of 10-200 μm; the suspending agent comprises guar gum, konjac glucomannan and artemisia glue; the mass ratio of guar gum, konjac glucomannan and artemisia glue in the suspending agent is 3:4: 4; the liquid phase component comprises the following components in parts by mass: 40 parts of solvent, wherein the solvent in the liquid phase component is glycerol, and the preparation method of the artemisia glue comprises the following steps: dissolving commercially available Artemisia desertorum gum powder in deionized water according to the ratio of 1:4-8 to prepare colloid, and grinding for 2-4h after vacuum freeze drying to obtain Artemisia desertorum gum powder.
9. A process for preparing a bone cement as claimed in any one of claims 1 to 7, wherein the calcium phosphate is mixed with the suspending agent to form a solid powder, the liquid component is added in proportion to form a paste, and the paste is stored in a sealed container at 4-50 ℃.
10. Use of a bone cement according to any of claims 1-7, characterised in that the filling is performed by direct injection by means of filling or by means of a syringe.
CN202110965388.9A 2021-08-23 2021-08-23 Anhydrous calcium phosphate bone cement and preparation method thereof Withdrawn CN113769159A (en)

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Application publication date: 20211210