CN104784752A - Injectable bone cement with antioxidation characteristic as well as preparation method and application thereof - Google Patents

Injectable bone cement with antioxidation characteristic as well as preparation method and application thereof Download PDF

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Publication number
CN104784752A
CN104784752A CN201510193933.1A CN201510193933A CN104784752A CN 104784752 A CN104784752 A CN 104784752A CN 201510193933 A CN201510193933 A CN 201510193933A CN 104784752 A CN104784752 A CN 104784752A
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bone cement
phosphate
beta
carotene
liquid
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CN201510193933.1A
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李朝阳
邸勋
崔永顺
吕维加
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Shandong Mingde Biomedical Engineering Co Ltd
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Shandong Mingde Biomedical Engineering Co Ltd
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Abstract

The invention discloses injectable bone cement with an antioxidation characteristic as well as a preparation method and application thereof. The bone cement consists of powder and liquid, wherein the powder consists of phosphate, sulfate and beta-carotene powder; the liquid consists of one or more of sodium citrate, sodium hydrogen phosphate and deionized water. The bone cement is prepared by using the preparation method which comprises the following steps: (1) uniformly mixing phosphate, sulfate, beta-carotene powder and a dispersing agent according to a mass ratio, wherein beta-carotene is 0.1-1% of the total mass and the dispersing agent is 0.01-0.3% of the total mass; (2) adding the solidified liquid to stir uniformly, wherein the proportion of the addition of the solidified liquid to the powder mixture prepared in the step (1) is 1.5-2.0 g/mL. The prepared bone cement has the characteristics of being injectable and high in strength, is capable of automatically and rapidly solidifying under physiological environment, and has good bioactivity, antioxidation characteristic and bone cell inducing characteristic.

Description

A kind of syringeability bone cement with anti-oxidation characteristics and its production and use
Technical field
The present invention relates to bone cement, be especially specifically related to a kind of syringeability bone cement with anti-oxidation characteristics and its production and use.
Background technology
The mark of osteoporosis is that bone density reduces, bone strength reduces, and it is the general bone metabolism disorder disease increasing to feature with risk of bone fracture; Wherein senile osteoporosis sickness rate is higher.Osteoporosis and osteoporotic fracture have become the serious public health social problem of worldwide concern, and Chinese existing patients with osteoporosis 9,000 ten thousand, accounts for 7.1% of total population; Along with the process of social senilization, the sickness rate of osteoporosis is still in rising trend, expects the year two thousand fifty will be increased to 2.21 hundred million, and osteoporotic fracture wherein about over half will occur in China.
Osteoporosis be the destruction of bone micro-structure at all, but osseous tissue has normal calcification, and calcium salt and substrate are normal rates, how slowly therefore fall ill, easily cause fracture.At present, clinically for osteoporotic fracture, the main fixing means adopting non-drug, but because the bone mass of patients with osteoporotic bone fracture is poor, be difficult to carry out effective internal fixtion, and fixed position elastic modelling quantity is comparatively large, thus increases the risk of adjacent sections generation refracture.
The topical therapeutic of osteoporosis and osteoporotic fracture is a kind of new technique means.By applying somatomedin and the biomaterial of osteosporosis resistant medicament or promoting bone growing at the position being easy to occur osteoporotic fracture, or directly fill above-mentioned material at fracture site, not only can reach the bone density improving local osteoporotic bone, the object improving bone micro-structure and bio-mechanical property, also avoid the internal fixtion problem of osteoporosis sample.
Apatite bone cement (Calcium phosphate cement, CPC) be a class novel, there is good biocompatibility and bioactive bone renovating material, can solidify voluntarily in physiological conditions, and can according to any plastotype in Cranial defect position also, its hydrated product hydroxyapatite is the host inorganic constituent of skeleton tissue.Also studies have found that, CPC has good biological degradability and bone conductibility, can in human body environment progressively degraded and absorbed being substituted by freshman bone tissue, overcome the deficiency from/bone renovating materials such as allograph bone, acrylic acid bone cement, bioceramic.But along with going deep into of research, conventional CPC has shown some shortcomings part, as very poor in mobility, curing rate is slow, mechanical strength is poor, degradation rate is low, these deficiencies have limited its application at more wide spectrum.At present, modification is carried out to CPC and just becoming one of emphasis of bio-medical material circle research to improve its physics and chemistry and biology performance.
The CPC cured product obtained by tetracalcium phosphate and calcium hydrogen phosphate system, calcium sulfate system is stoichiometric hydroxyapatite (HAP), its calcium-phosphorus ratio (Ca/P) is 1.67, degradable and absorption in vivo, but syringeability is poor, under pressurized condition, there will be solid-liquid separation; In order to improve its injection property, adding surfactant and improving bonding state between powder liquid, the good CPC powder of mobility can be obtained.
Beta-carotene has the title of vitamin a source, is a kind of important human body physiological function active substance.In recent years, about beta-carotene is to the research Showed Very Brisk of human body effect.Large quantity research confirms; many biological functions of beta-carotene and human health have substantial connection; it is at antioxidation, removing toxic substances, anticancer, angiocardiopathy preventing, and the physiological action of preventing and treating cataract and the liver protecting aspect is confirmed more and more and is applied to prevention and treatment of diseases.Research shows, beta-carotene reduces its injury effect to cell by the combination with free radical.
Up to the present, the work carrying out studying and exploring for the syringeability bone cement both combined have not been reported.
Summary of the invention
Technical problem to be solved by this invention is, in order to the defect overcoming existing bone cement poor fluidity, mechanical strength is not suitable for, biocompatibility is to be improved, degradation speed is too slow, and a kind of good flowing properties is provided, mechanical strength is suitable for, good biocompatibility, degradation property are excellent is used for the treatment of syringeability bone cement with anti-oxidation characteristics of osteoporotic fracture and its production and use.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of syringeability bone cement with anti-oxidation characteristics, bone cement is made up of powder body and liquid, powder body comprises sulfate, phosphate, dispersant and beta-carotene, and beta-carotene accounts for the 0.1%-1% of bone cement powder body gross mass.
Described liquid is one or more compositions in sodium citrate, dibastic sodium phosphate and deionized water.
Described dispersant is the one or more combination in polyvinylpyrrolidone, Polyethylene Glycol, carboxymethyl cellulose and polyvinyl alcohol, and described dispersant accounts for the 0.01%-0.3% of bone cement powder body gross mass.
Described phosphate is one or more in tetracalcium phosphate, tricalcium phosphate, calcium hydrogen phosphate, and sulfate is one or both compositions in half-H 2 O calcium sulphate and calcium sulfate.
The above-mentioned preparation method with the syringeability bone cement of anti-oxidation characteristics, comprises the steps:
(1) by sulfate, phosphate and beta-carotene powder body and dispersant mix homogeneously in mass ratio, wherein beta-carotene accounts for the 0.1%-1% of powder body gross mass, and dispersant accounts for the 0.01%-0.3% of powder body gross mass;
(2) add the liquid agitation of solidification evenly, powder mixture prepared in the addition of the liquid of solidification and step (1) is than being 1.5g/mL-2.0g/mL.
The liquid of described solidification is deionized water.
The above-mentioned syringeability bone cement with anti-oxidation characteristics, as the purposes in bone renovating material.
The invention has the beneficial effects as follows: injecting bone cement of the present invention has good fluidity, fast solidifying feature, Wicresoft can inject, and solidify voluntarily under physiological environment, hardening time is short, comprcssive strength is close to spongy bone demand, and cured product is mainly hydroxyapatite.
Accompanying drawing explanation
Fig. 1 is the comprcssive strength figure of antioxidation biology active bone cement of the present invention.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail:
The syringeability bone cement with anti-oxidation characteristics of the present invention, bone cement is made up of powder body and liquid, and powder body comprises sulfate, phosphate, dispersant and beta-carotene, and beta-carotene accounts for the 0.1%-1% of bone cement powder body gross mass.
Described liquid is one or more compositions in sodium citrate, dibastic sodium phosphate and deionized water.
Described dispersant is the one or more combination in polyvinylpyrrolidone, Polyethylene Glycol, carboxymethyl cellulose and polyvinyl alcohol, and described dispersant accounts for the 0.01%-0.3% of bone cement powder body gross mass.
Described phosphate is one or more in tetracalcium phosphate, tricalcium phosphate, calcium hydrogen phosphate, and sulfate is one or both compositions in half-H 2 O calcium sulphate and calcium sulfate.
The above-mentioned preparation method with the syringeability bone cement of anti-oxidation characteristics, comprises the steps:
(1) by sulfate, phosphate and beta-carotene powder body and dispersant mix homogeneously in mass ratio, wherein beta-carotene accounts for the 0.1%-1% of powder body gross mass, and dispersant accounts for the 0.01%-0.3% of powder body gross mass;
(2) add the liquid agitation of solidification evenly, powder mixture prepared in the addition of the liquid of solidification and step (1) is than being 1.5g/mL-2.0g/mL.
The liquid of described solidification is deionized water.
The above-mentioned syringeability bone cement with anti-oxidation characteristics, as the purposes in bone renovating material.
The present invention prepares Wicresoft's injecting bone cement, makes it have Bone Defect Repari function, for preventing and treating osteoporotic fracture.Injectable materials, while reparation bone, also can promote new bone formation, thus control osteoporotic fracture; The micropore of bone cement material is conducive to growing into of osteocyte/tissue, thus improves the degradability of material, promotes Bone Defect Repari.
The present invention adds antioxidant beta-carotene, reaches the osseous tissue that prevents from contacting with bone cement and bone surrounding tissue is aging and the old and feeble disease caused; Its metabolite vitamin A has promoting growth of cell ability, has facilitation to the growth of new bone, thus promotes that osseous tissue is grown into.
Described dispersant is that this area is conventional, and consumption is that this area is conventional, and preferably, the consumption of described dispersant is the 0.01%-0.3% accounting for described CPC powder quality.
Mode below by embodiment further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments.The experimental technique of unreceipted actual conditions in the following example, conventionally and condition.
The syringeability bone cement of embodiment 1-4 antioxidation biology activity and the preparation of slurry thereof:
Bone cement powder is prepared by the tetracalcium phosphate of 1 ︰ 2 and calcium hydrogen phosphate, appropriate other phosphate, sulfate and beta-carotene, dispersant by mol ratio, wherein Beta Carotene Powder quality accounts for 0.1%-1%, and the consumption of dispersant is the 0.01%-0.3% accounting for CPC quality.
In embodiment, the composition of bone cement powder used is in table 1.Four kinds of bone cements all adopt deionized water to be consolidation liquid.
The composition of several bone cement powder of table 1
Note: gross mass is 100%
Embodiment 5 performance test
1, the mensuration of setting time
Cement consistency and coagulation time tester is adopted to measure the setting time of bone cement slurry.
Mixed homogeneously by a certain percentage with consolidation liquid by bone cement powder, high H=10mm made by the cement mortar be in harmonious proportion, and the sample of diameter D=6mm puts into 37 DEG C after the demoulding, solidify, take out at set intervals in 100% humidity environment.During mensuration, be placed in by sample on glass plate and test point is contacted with slurry face, loosen screw suddenly, test point freely sinks to slurry, observes pointer instruction numerical value.Be defined as setting time from be in harmonious proportion powder and sink to slurry to test point and be no more than the time that 1mm experiences.
2, the mensuration of comprcssive strength
Mixed homogeneously by a certain percentage with consolidation liquid by bone cement powder, the cement mortar be in harmonious proportion is put into stainless steel mould and is made high H=12mm, the sample of diameter D=6mm, flattens with the weight of 2kg to drive bubble away as far as possible.Take out the batten after pressing through, put into 37 DEG C, solidify certain hour in 100% humidity environment, two ends polish, and measure comprcssive strength with material mechanical performance universal testing machine, imposed load speed is 1mm/min, often organize data at least three parallel laboratory tests.
3, porosity measurement
Prepare the sample of regular shape and suitable size, put into 37 DEG C of pure water and flood 24h after measuring its diameter D, height H and dry weight M1, weigh after taking out wipe surfaces moisture M2, the quality of water in weightening finish and space, volume shared by it and pore volume.Often organize at least three Duplicate Samples.
4, the mensuration of external degradation performance
This experiment adopts phosphate buffer solution (PBS) to evaluate the degradability of bone cement firming body.By bone cement firming body sample vacuum drying, its first weight (W0) of accurate weighing, record, numbering.Again sample is immersed in PBS and be placed in 37 DEG C, vibrate in the constant temperature oscillation case of rotating speed 100r/min, within every 48 hours, change PBS once, total immersion bubble 12 weeks.Regular taking-up sample, sucks moisture with filter paper, and weigh after vacuum drying (Wt), and observe the metamorphosis of sample.
Weight-loss ratio according to formulae discovery sample below: weight-loss ratio=(W0-Wt)/W0 × 100%, often organizes 3 Duplicate Samples, averages.
5, after degraded, pH value measures
Several bone cement samples of solidification after 24 hours are immersed in SBF respectively, are placed in 37 DEG C, vibrate in the constant temperature oscillation case of rotating speed 100r/min, after 1 hour, 12 hours, 48 hours, 5 days, 7 days, measure the pH value of solution in immersion with pH meter respectively.
Can learn from result, the content of beta-carotene has obvious impact the hardening time on bone cement, beta-carotene add the hardening time extending common calcium sulfate calcium phosphate bone cement; Along with the reduction of content, the setting time of bone cement shortens gradually, the content of beta-carotene 0.1% time hardening time about 15min.
The comprcssive strength of content to firming body of beta-carotene also has certain influence, beta-carotene add the compressive strength reducing common calcium sulfate calcium phosphate bone cement, be about about 2MPa.
Adding of dispersant effectively improves the present situation that apatite bone cement fluidity is poor, injectivity is poor; After being mixed into slurry, viscoelasticity is better, good flowing properties, and adding pressure does not have obvious solid-liquid separation, injectable;
After bone cement solidification prepared by the present invention, through-hole rate is high, can reach more than 20%.
Degradation speed is moderate, degradable about 4% after 24h, within 11 weeks, can reach 60%-70%.The pH of degradation solution between 6.0-6.8, in faintly acid.
The comprcssive strength of gained sample in the corresponding embodiment 1-4 of difference shown in Fig. 1, the comprcssive strength of the active injecting bone cement of the antioxidation biology prepared as seen from the figure is all at more than 2MPa.
On the basis meeting this area general knowledge, above-mentioned each optimum condition, can combination in any, obtains the preferred embodiments of the invention.
Above-described embodiment is only for illustration of technological thought of the present invention and feature, its object is to enable those skilled in the art understand content of the present invention and implement according to this, only can not limit the scope of the claims of the present invention with the present embodiment, namely the equal change done of all disclosed spirit or modification, still drop in the scope of the claims of the present invention.

Claims (7)

1. have a syringeability bone cement for anti-oxidation characteristics, it is characterized in that, bone cement is made up of powder body and liquid, and powder body comprises sulfate, phosphate, dispersant and beta-carotene, and beta-carotene accounts for the 0.1%-1% of bone cement powder body gross mass.
2. the syringeability bone cement with anti-oxidation characteristics according to claim 1, is characterized in that, described liquid is one or more compositions in sodium citrate, dibastic sodium phosphate and deionized water.
3. the syringeability bone cement with anti-oxidation characteristics according to claim 1, it is characterized in that, described dispersant is the one or more combination in polyvinylpyrrolidone, Polyethylene Glycol, carboxymethyl cellulose and polyvinyl alcohol, and described dispersant accounts for the 0.01%-0.3% of bone cement powder body gross mass.
4. the syringeability bone cement with anti-oxidation characteristics according to claim 1, it is characterized in that, described phosphate is one or more in tetracalcium phosphate, tricalcium phosphate, calcium hydrogen phosphate, and sulfate is one or both compositions in half-H 2 O calcium sulphate and calcium sulfate.
5. there is a preparation method for the syringeability bone cement of anti-oxidation characteristics as claimed in claim 1, it is characterized in that, comprise the steps:
(1) by sulfate, phosphate and beta-carotene powder body and dispersant mix homogeneously in mass ratio, wherein beta-carotene accounts for the 0.1%-1% of powder body gross mass, and dispersant accounts for the 0.01%-0.3% of powder body gross mass;
(2) add the liquid agitation of solidification evenly, powder mixture prepared in the addition of the liquid of solidification and step (1) is than being 1.5g/mL-2.0g/mL.
6. the preparation method with the syringeability bone cement of anti-oxidation characteristics according to claim 5, is characterized in that, the liquid of described solidification is deionized water.
7. there is the syringeability bone cement of anti-oxidation characteristics as claimed in claim 1, as the purposes in bone renovating material.
CN201510193933.1A 2015-04-22 2015-04-22 Injectable bone cement with antioxidation characteristic as well as preparation method and application thereof Pending CN104784752A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105031738A (en) * 2015-09-09 2015-11-11 山东明德生物医学工程有限公司 Weak-exothermic bone cement and preparation method and application
CN105396178A (en) * 2015-11-20 2016-03-16 山东明德生物医学工程有限公司 Injectable antibacterial bone cement
CN105536070A (en) * 2016-02-05 2016-05-04 山东明德生物医学工程有限公司 Composite bone cement and preparation method thereof
CN109125804A (en) * 2018-10-18 2019-01-04 暨南大学 A kind of solidify liquid and the preparation method and application thereof suitable for calcium orthophosphate base bone cement

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090324669A1 (en) * 2006-07-26 2009-12-31 The Regents Of The University Of California Osteogenic enhancer composition
CN103379923A (en) * 2010-07-02 2013-10-30 阿格诺沃医疗保健有限责任公司 Composition comprising calcium phosphate and sulfate powders and tri-calcium phosphate particles used in the treatment of degenerative bone conditions
CN104056305A (en) * 2014-04-24 2014-09-24 安泰科技股份有限公司 Calcium phosphate-based compound self-setting bone repair material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090324669A1 (en) * 2006-07-26 2009-12-31 The Regents Of The University Of California Osteogenic enhancer composition
CN103379923A (en) * 2010-07-02 2013-10-30 阿格诺沃医疗保健有限责任公司 Composition comprising calcium phosphate and sulfate powders and tri-calcium phosphate particles used in the treatment of degenerative bone conditions
CN104056305A (en) * 2014-04-24 2014-09-24 安泰科技股份有限公司 Calcium phosphate-based compound self-setting bone repair material and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105031738A (en) * 2015-09-09 2015-11-11 山东明德生物医学工程有限公司 Weak-exothermic bone cement and preparation method and application
CN105396178A (en) * 2015-11-20 2016-03-16 山东明德生物医学工程有限公司 Injectable antibacterial bone cement
CN105536070A (en) * 2016-02-05 2016-05-04 山东明德生物医学工程有限公司 Composite bone cement and preparation method thereof
CN109125804A (en) * 2018-10-18 2019-01-04 暨南大学 A kind of solidify liquid and the preparation method and application thereof suitable for calcium orthophosphate base bone cement
CN109125804B (en) * 2018-10-18 2021-03-19 暨南大学 Curing liquid suitable for calcium phosphate-based bone cement and preparation method and application thereof

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