CN103656743A - Bone cement having solid-liquid separation resistance, and preparation method thereof - Google Patents
Bone cement having solid-liquid separation resistance, and preparation method thereof Download PDFInfo
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- CN103656743A CN103656743A CN201310641572.3A CN201310641572A CN103656743A CN 103656743 A CN103656743 A CN 103656743A CN 201310641572 A CN201310641572 A CN 201310641572A CN 103656743 A CN103656743 A CN 103656743A
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Abstract
The invention relates to a bone cement having a solid-liquid separation resistance, and a preparation method thereof. The preparation method comprises the following steps: preparing a citric acid-chitosan solution containing 3-55% of citric acid and 0.05-10% of chitosan; preparing a solidification liquid containing 0.01-10% of gelatin, 0.01-10% of hydroxypropyl methyl cellulose and other additives on the basis of the citric acid-chitosan solution; preserving the solidification liquid in 4DEG C environment if the solidification is not used for a long term, and pre-dissolving before use; and blending bone cement powder with the solidification liquid according to a liquid/solid ratio to obtain the bone cement having a solid-liquid separation resistance. Each of the bone cement and the solidification liquid has the advantages of wide sources and low prices of components, and good commercialization prospect. The solidification liquid has the advantages of simple and feasible operation, good effect, suitableness for the wide use in organic calcium-based bone cement systems, and large scale application.
Description
Technical field
The present invention relates to a kind of method of bio-medical material technical field, specifically a kind of bone cement that has good anti-solid-liquid separation characteristic and preparation method thereof.
Background technology
When bone cement is repaired for bone, its mechanical strength of General Requirements at least reaches degree 0.4 ~ 30.0 MPa [Miao Jun, Wang Jifang, Chinese Reconstructive surgery magazine, 2005] of Human cancellous bone.Calcium phosphate bone cement is repaired field because the advantages such as its good biocompatibility, osteoinductive, degradable are widely used in bone.Bone cement is generally comprised of powder and consolidation liquid two parts.In common consolidation liquid, conventionally contain the compositions such as sodium hydrogen phosphate, sodium dihydrogen phosphate, citric acid.In order to improve bone cement mechanical strength, tend to add reinforcing agent and comprise [Han Bing etc., Materials Science and Engineering, 2006] such as fiber, gelatin, chitosan, poly (glycolide-lactide) (PLGA), hydroxyapatite crystal whisker, inorganic ceramic granules.
The curable molding although a lot of bone cement powder and consolidation liquid are filled a prescription, conventionally can be separated with consolidation liquid because issue green powder in large injection extruding force when actual medical is applied, and causes operative failure.Possible reason is that before the composition in powder and consolidation liquid solidifies, adhesion is strong not, causes occurring under external force serious macroface separated.
Summary of the invention
The object of the present invention is to provide a kind of method of bio-medical material technical field, specifically a kind of bone cement that has good anti-solid-liquid separation characteristic and preparation method thereof.By allocating rightly consolidation liquid, fill a prescription, a kind of bone cement that has good anti-solid-liquid separation characteristic and preparation method thereof is provided.
Object of the present invention is achieved through the following technical solutions: citric acid, chitosan, gelatin, hydroxypropyl emthylcellulose and other additives are mixed by a certain percentage, obtain a kind of novel consolidation liquid; Consolidation liquid and bone cement powder are in harmonious proportion by certain liquid-solid ratio, can obtain having the bone cement of good anti-solid-liquid separation characteristic.
A preparation method with the bone cement of anti-solid-liquid separation characteristic, is characterized in that, comprises the following steps:
(1) preparation citric acid-chitosan solution, wherein citric acid content is 3-55%, chitosan content is 0.05-10%;
(2) consolidation liquid that preparation contains 0.01-10% gelatin, 0.01-10% hydroxypropyl emthylcellulose and other additives on the basis of citric acid-chitosan solution;
(3) if consolidation liquid for a long time need not, be stored in 4 ℃ of environment, molten in advance before use;
(4) bone cement powder and consolidation liquid are in harmonious proportion by liquid-solid ratio, can obtain having the bone cement of anti-solid-liquid separation characteristic.
The solvent of citric acid-chitosan solution that step (1) is described is aqueous solution, or acid solution.
Described acid solution is a kind of or its combination in 0.01-0.3 M hydrochloric acid solution, 0.01-0.3 M sulfuric acid solution, 0.01-0.5 M phosphoric acid solution, 0.01-0.6 M acetic acid solution, 0.01-0.2 M salpeter solution, 0.01-0.5 M ascorbic acid solution, 0.01-0.5 M lactic acid solution.
The manner of formulation of the solution that step (1) is described is that room temperature is dissolved, or 60 ℃ of following heating hydrotropies, can also be aided with mechanical agitation or magnetic agitation.
The sodium carboxymethyl cellulose that other additives in consolidation liquid described in step (2) are 0.01-2%, 0.01-1.5% polyvinyl alcohol, 0.01-10% Polyethylene Glycol, 0.01-2% sodium alginate, 0.01-5% starch, 0.01-1% hyaluronic acid, 0.01-2% collagen protein, 0.5-40% glycerol, 0.01-15% sodium sulfate, 0.01-15% potassium sulfate, 0.01-15% ammonium sulfate, 0.01-10% magnesium sulfate, 0.01-10% sodium chloride, 0.01-10% potassium chloride, 0.01-15% calcium chloride, 0.01-15% sodium glycerophosphate, 0.01-15% glucose, 0.01-15% mannose, a kind of or its combination in 0.01-5% cyclodextrin.
The described pre-molten mode of step (3) is to make consolidation liquid become flowable liquid 37 ℃ of following heating.
The described liquid-solid ratio of step (4) is in every 1 gram of bone cement powder, to add the consolidation liquid of 0.30-0.70 milliliter.
The bone cement with anti-solid-liquid separation characteristic preparing according to method described in above-mentioned any one; When pressure is greater than 5 MPa, without solid-liquid separation phenomenon, injectability coefficient is not less than 80%, be no more than 40 minutes hardening time.
Consolidation liquid formula provided by the invention can keep injectivity and anti-solid-liquid separation characteristic that bone cement is good under larger pressure.Meanwhile, in consolidation liquid, contain the bone cement reinforcing agents such as chitosan, gelatin, hydroxypropyl emthylcellulose.In the anti-solid-liquid separation improving under its high pressure, can improve its comprcssive strength again.Method provided by the invention is simple, easily capable, effective, be suitable for promoting the use of in the inorganic calcio bone cement of difference system, can large-scale application.
Injectability coefficient testing method is: the bone cement that is no less than 3 mL being in harmonious proportion is inserted in disposable syringe, with constant rate of speed, promote, extremely maximum propulsive force is that 100 N stop, and the percentage ratio that the bone cement weight of release is accounted for to bone cement gross weight is as injectability coefficient.
The specific embodiment
Following examples be take invention technical scheme and are implemented as prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention are not limited to following embodiment.
Embodiment 1:
Take 86 g calcium phosphate dibasic dihydrates and 25 g calcium carbonate, joined ball milling mix homogeneously in 165 mL water.Then by water distilling under reduced pressure, in 80 ℃ of vacuum drying ovens, be dried and obtain mixed powder.After burning 15 hours, 900 ℃ of stove stage casings adopt wet ball grinding to obtain bone cement dispersion liquid powder body.After dispersion liquid is centrifugal, dry, obtain bone cement powder main body composition.91 g bone cement powder main body compositions, 4 g hydroxyapatite and 5 g sodium sulfate are ground and evenly obtain bone cement powder with mortar.
Embodiment 2:
Take 20.0 g citric acids, 1.0 g chitosans, 1.0 g gelatin, 1.0 g hydroxypropyl emthylcelluloses, 3.0 g glycerol and be dissolved in 74 mL water, obtain consolidation liquid.Bone cement consolidation liquid and powder are in harmonious proportion by the liquid-solid ratio of 0.5 mL/g, and it is 15 min that reference standard ASTM C191 measures the presetting period.The bone cement slurry being in harmonious proportion proceeds to and in injector for medical purpose, shows good injectivity.Injectability coefficient is 96%, under 5 MPa pressure without solid-liquid separation phenomenon.
Embodiment 3:
Take 20.0 g citric acids, 1.0 g chitosans, 1.0 g gelatin, 1.0 g hydroxypropyl emthylcelluloses, 10 g glycerol and be dissolved in 67 mL water, obtain consolidation liquid.Bone cement consolidation liquid and powder are in harmonious proportion by the liquid-solid ratio of 0.5 mL/g, and it is 25 min that reference standard ASTM C191 measures the presetting period.The bone cement slurry being in harmonious proportion is proceeded to and in injector for medical purpose, shows good injectivity.Injectability coefficient is 95%, under 5 MPa pressure without solid-liquid separation phenomenon.
Claims (8)
1. a preparation method with the bone cement of anti-solid-liquid separation characteristic, is characterized in that, comprises the following steps:
(1) preparation citric acid-chitosan solution, wherein citric acid content is 3-55%, chitosan content is 0.05-10%;
(2) consolidation liquid that preparation contains 0.01-10% gelatin, 0.01-10% hydroxypropyl emthylcellulose and other additives on the basis of citric acid-chitosan solution;
(3) if consolidation liquid for a long time need not, be stored in 4 ℃ of environment, molten in advance before use;
(4) bone cement powder and consolidation liquid are in harmonious proportion by liquid-solid ratio, can obtain having the bone cement of anti-solid-liquid separation characteristic.
2. have according to claim 1 the preparation method of the bone cement of anti-solid-liquid separation characteristic, it is characterized in that, the solvent of citric acid-chitosan solution that step (1) is described is aqueous solution, or acid solution.
3. there is according to claim 2 the preparation method of the bone cement of anti-solid-liquid separation characteristic, it is characterized in that, described acid solution is a kind of or its combination in 0.01-0.3 M hydrochloric acid solution, 0.01-0.3 M sulfuric acid solution, 0.01-0.5 M phosphoric acid solution, 0.01-0.6 M acetic acid solution, 0.01-0.2 M salpeter solution, 0.01-0.5 M ascorbic acid solution, 0.01-0.5 M lactic acid solution.
4. have according to claim 1 the preparation method of the bone cement of anti-solid-liquid separation characteristic, it is characterized in that, the manner of formulation of the solution that step (1) is described is that room temperature is dissolved, or 60 ℃ of following heating hydrotropies, can also be aided with mechanical agitation or magnetic agitation.
5. there is according to claim 1 the preparation method of the bone cement of anti-solid-liquid separation characteristic, it is characterized in that, the sodium carboxymethyl cellulose that other additives in consolidation liquid described in step (2) are 0.01-2%, 0.01-1.5% polyvinyl alcohol, 0.01-10% Polyethylene Glycol, 0.01-2% sodium alginate, 0.01-5% starch, 0.01-1% hyaluronic acid, 0.01-2% collagen protein, 0.5-40% glycerol, 0.01-15% sodium sulfate, 0.01-15% potassium sulfate, 0.01-15% ammonium sulfate, 0.01-10% magnesium sulfate, 0.01-10% sodium chloride, 0.01-10% potassium chloride, 0.01-15% calcium chloride, 0.01-15% sodium glycerophosphate, 0.01-15% glucose, 0.01-15% mannose, a kind of or its combination in 0.01-5% cyclodextrin.
6. have according to claim 1 the preparation method of the bone cement of anti-solid-liquid separation characteristic, it is characterized in that, the described pre-molten mode of step (3) is to make consolidation liquid become flowable liquid 37 ℃ of following heating.
7. have according to claim 1 the preparation method of the bone cement of anti-solid-liquid separation characteristic, it is characterized in that, the described liquid-solid ratio of step (4) is in every 1 gram of bone cement powder, to add the consolidation liquid of 0.30-0.70 milliliter.
8. the bone cement with anti-solid-liquid separation characteristic preparing according to method described in claim 1-7 any one; When pressure is greater than 5 MPa, without solid-liquid separation phenomenon, injectability coefficient is not less than 80%, be no more than 40 minutes hardening time.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104027838A (en) * | 2014-05-28 | 2014-09-10 | 上海纳米技术及应用国家工程研究中心有限公司 | Fast-curing sodium citrate and carboxylation chitosan reinforced bone cement and preparation method thereof |
| CN104368042A (en) * | 2014-11-19 | 2015-02-25 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of brushite bone cement |
| CN104491924A (en) * | 2015-01-05 | 2015-04-08 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of injectable medicine-carrying brushite bone cement |
| CN104591679A (en) * | 2015-01-31 | 2015-05-06 | 河南理工大学 | Modified magnesium oxychloride bone cement as well as preparation method and application thereof |
| CN105251058A (en) * | 2015-11-05 | 2016-01-20 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing drug-loaded injection type calcium sulfate bone cement for promoting bone growth |
| CN106031799A (en) * | 2015-03-12 | 2016-10-19 | 中国科学院理化技术研究所 | Calcium silicate/strontium salt bone cement and preparing method thereof |
| CN106267365A (en) * | 2016-08-17 | 2017-01-04 | 林春梅 | A kind of enhancing activity injecting bone cement and preparation method thereof |
| CN109939261A (en) * | 2019-04-24 | 2019-06-28 | 东南大学 | A kind of solidify liquid and its preparation method and application of controllable calcium phosphate bone cement injectivity |
| CN111991615A (en) * | 2020-08-11 | 2020-11-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of lanthanide-doped injectable calcium phosphate bone cement, product and application thereof |
| CN113144292A (en) * | 2021-03-11 | 2021-07-23 | 苏州大学 | Stem cell secretion, preparation method thereof, bioactive bone cement, preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104027838A (en) * | 2014-05-28 | 2014-09-10 | 上海纳米技术及应用国家工程研究中心有限公司 | Fast-curing sodium citrate and carboxylation chitosan reinforced bone cement and preparation method thereof |
| CN104368042A (en) * | 2014-11-19 | 2015-02-25 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of brushite bone cement |
| CN104491924A (en) * | 2015-01-05 | 2015-04-08 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of injectable medicine-carrying brushite bone cement |
| CN104591679A (en) * | 2015-01-31 | 2015-05-06 | 河南理工大学 | Modified magnesium oxychloride bone cement as well as preparation method and application thereof |
| CN106031799A (en) * | 2015-03-12 | 2016-10-19 | 中国科学院理化技术研究所 | Calcium silicate/strontium salt bone cement and preparing method thereof |
| CN105251058B (en) * | 2015-11-05 | 2018-07-17 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method for carrying medicine and promoting bone uptake injection-type calcium sulfate bone cement |
| CN105251058A (en) * | 2015-11-05 | 2016-01-20 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing drug-loaded injection type calcium sulfate bone cement for promoting bone growth |
| CN106267365A (en) * | 2016-08-17 | 2017-01-04 | 林春梅 | A kind of enhancing activity injecting bone cement and preparation method thereof |
| CN109939261A (en) * | 2019-04-24 | 2019-06-28 | 东南大学 | A kind of solidify liquid and its preparation method and application of controllable calcium phosphate bone cement injectivity |
| CN109939261B (en) * | 2019-04-24 | 2021-06-11 | 东南大学 | Curing liquid capable of regulating and controlling injection property of calcium phosphate bone cement and preparation method and application thereof |
| CN111991615A (en) * | 2020-08-11 | 2020-11-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of lanthanide-doped injectable calcium phosphate bone cement, product and application thereof |
| CN113144292A (en) * | 2021-03-11 | 2021-07-23 | 苏州大学 | Stem cell secretion, preparation method thereof, bioactive bone cement, preparation method and application |
| CN113144292B (en) * | 2021-03-11 | 2021-12-21 | 苏州大学 | Stem cell secretion, preparation method thereof, bioactive bone cement, preparation method and application |
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Application publication date: 20140326 |