CN103690990A - Collapse-resistance injection neutral bone cement and preparation method thereof - Google Patents
Collapse-resistance injection neutral bone cement and preparation method thereof Download PDFInfo
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- CN103690990A CN103690990A CN201310641545.6A CN201310641545A CN103690990A CN 103690990 A CN103690990 A CN 103690990A CN 201310641545 A CN201310641545 A CN 201310641545A CN 103690990 A CN103690990 A CN 103690990A
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Abstract
The invention relates to collapse-resistance injection neutral bone cement and a preparation method thereof. The preparation method comprises the following steps: preparing citric solution with concentration of 3-55 percent; preparing sodium carboxymethylcellulose modified curing liquid with concentration of 0.01-2 percent based on the citric acid solution; storing the curing liquid in a 4 DEG C environment if the curing liquid is not used for a long time; and pre-dissolving before the curing liquid is used; and mixing the bone cement powder and the curing liquid according to a liquid-solid ratio to obtain the collapse-resistance injection neutral bone cement. Common defects of easy collapse, imperfect injection effect and strong acidity of bone cement in similar systems can be overcome, and the application range of related systems can be enlarged. The preparation method is simple, practical and good in effect, is suitable for popularization and application in different bone cement systems, and can be applied in a large scale.
Description
Technical field
The present invention relates to a kind of method of bio-medical material technical field, specifically a kind of anti-collapsibility, the neutral bone cement of injectable and preparation method thereof.
Background technology
Calcium phosphate bone cement (CPC) has the advantages such as good biocompatibility, bone conductibility, degradability and plasticity because of it, be widely used in new type bone repair materials, be subject to lot of domestic and foreign scholar's extensive concern ［ Han Bing etc., chemical industry progress, 2006 ］.
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.The material that tends to interpolation enhancing in order to improve bone cement intensity comprises [Han Bing etc., Materials Science and Engineering, 2006] such as fiber, gelatin, chitosan, poly (glycolide-lactide) (PLGA), hydroxyapatite crystal whisker, inorganic ceramic granules.Wherein, sodium carboxymethyl cellulose is due to wide material sources, be significantly subject to increasing attention to bone cement modified effect, and the bone cement of sodium carboxymethyl cellulose modification has the potentiality of suitability for industrialized production.
When bone cement is repaired for bone, good anti-collapsibility and syringeability are the primary conditions [Tao Yan, Li Dongxu, Li Yanbao, material Leader A: a summary piece of writing, 2011] of bone cement application.While being used for solidifying bone cement, often there is the deficiencies such as anti-collapsibility is poor, mechanical strength is undesirable in common consolidation liquid.In addition, the consolidation liquid that contains citric acid also exists bone cement to be highly acid shortcoming, has seriously limited it and has further applied.
The present invention is directed to above background with not enough, a kind of anti-collapsibility, the neutral bone cement of injectable and preparation method thereof are provided, by regulation and control bone cement powder powder formulation and consolidation liquid composition, prepared a kind of anti-collapsibility, the neutral bone cement of injectable.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of anti-collapsibility, the neutral bone cement of injectable and preparation method thereof are provided.Object of the present invention is achieved through the following technical solutions: a certain proportion of calcium hydrogen phosphate is fully mixed with calcium carbonate powder; Then adopt the method for solid state reaction, by controlling rightly reaction condition, prepare bone cement powder main body composition.On this basis toward adding a certain amount of hydroxyapatite in powder and the abundant mix homogeneously of silicate is prepared bone cement powder.By citric acid and the sodium carboxymethyl cellulose water-soluble bone cement consolidation liquid of preparing by a certain percentage.Bone cement powder and consolidation liquid are in harmonious proportion by certain liquid-solid ratio, can obtain hardening time rationally, anti-collapsibility, the neutral bone cement of injectable.
A preparation method for the neutral bone cement of anti-collapsibility injectable, is characterized in that, comprises the following steps:
(1) citric acid solution that compound concentration is 3-55%;
(2) consolidation liquid of the sodium carboxymethyl cellulose modification that compound concentration is 0.01-2% on the basis of citric acid 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 the neutral bone cement of anti-collapsibility injectable.
The solvent of the citric acid solution that step (1) is described can be 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 citric acid solution that step (1) is described is that room temperature is dissolved or ultrasonic dissolution assisting, can also be aided with mechanical agitation or magnetic agitation.
The manner of formulation of the consolidation liquid of the sodium carboxymethyl cellulose modification that step (2) is described is that room temperature is dissolved, or ultrasonic dissolution assisting, can also be aided with mechanical agitation or magnetic agitation.
The described pre-molten mode of step (3) is 37 ℃ of mobility that add below the consolidation liquid of heat gain sodium carboxymethyl cellulose modification.
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 neutral bone cement of anti-collapsibility injectable preparing according to method described in above-mentioned any one; Its pH value in water is 5-9, and defeated and dispersed coefficient is not more than 1%, and injectability coefficient is not less than 35%.
The present invention is directed to the deficiencies in the prior art, by the preparation technology of regulation and control bone cement powder and the formula of consolidation liquid, form, overcome that this type of system common anti-collapsibility, syringeability are undesirable, the acid deficiency such as stronger of bone cement, expanded the range of application of related system.Preparation method provided by the invention is simple, easily capable, effective, be suitable for promoting the use of in different bone cement systems, 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 method of testing of defeated and dispersed coefficient is: after solidifying, bone cement soaks after 10 days quality and reduces percentage ratio as defeated and dispersed coefficient in water.
PH value method of testing containing bone cement aqueous solution is: the bone cement that 1.0 g were solidified after 24 hours is placed in 20 mL ultra-pure waters, then with pH meter, measures it at the pH value of different soak times.
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 powder main body composition powder body.96 g bone cement powder main body compositions are mixed homogeneously and obtained bone cement powder with 4 g hydroxyapatite.
Embodiment 2:
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 degree 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 powder main body composition powder body.91 g bone cement powder main body compositions are mixed homogeneously and obtained bone cement powder with 4 g hydroxyapatite and 5 g sodium silicate.
Embodiment 3:
Take 1.0 g sodium carboxymethyl cellulose and join in 99 mL 20% aqueous citric acid solutions and dissolve, obtain the consolidation liquid of sodium carboxymethyl cellulose modification.Bone cement powder in embodiment 1 and consolidation liquid are in harmonious proportion by the liquid-solid ratio of 0.5 mL/g, and it is 8 min that reference standard ASTM C191 measures the presetting period.By the bone cement piece after solidifying put into water after 30 days without obvious defeated and dispersed phenomenon, solution is also neutrality always.After solidifying, bone cement is placed after 30 days and is still kept original form in water, and defeated and dispersed coefficient is 0.8%.When bone cement is extruded in water with syringe, bone cement does not disintegrate in water.Its injectability coefficient is 50%.
Embodiment 4:
Take 1.0 g sodium carboxymethyl cellulose and join in 99 mL 20% aqueous citric acid solutions and dissolve, obtain the consolidation liquid of sodium carboxymethyl cellulose modification.Bone cement consolidation liquid in embodiment 2 and powder are in harmonious proportion by the liquid-solid ratio of 0.5 mL/g, and it is 10 min that reference standard ASTM C191 measures the presetting period.By the bone cement piece after solidifying put into water after 30 days without obvious defeated and dispersed phenomenon, in water, solution is neutrality always, defeated and dispersed coefficient is 0.9%.
Claims (8)
1. a preparation method for the neutral bone cement of anti-collapsibility injectable, is characterized in that, comprises the following steps:
(1) citric acid solution that compound concentration is 3-55%;
(2) consolidation liquid of the sodium carboxymethyl cellulose modification that compound concentration is 0.01-2% on the basis of citric acid 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 the neutral bone cement of anti-collapsibility injectable.
2. the preparation method of the neutral bone cement of anti-collapsibility injectable according to claim 1, is characterized in that, the solvent of the citric acid solution that step (1) is described can be aqueous solution, or acid solution.
3. the preparation method of the neutral bone cement of anti-collapsibility injectable according to claim 2, 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. the preparation method of the neutral bone cement of anti-collapsibility injectable according to claim 1, is characterized in that, the manner of formulation of the citric acid solution that step (1) is described is that room temperature is dissolved or ultrasonic dissolution assisting, can also be aided with mechanical agitation or magnetic agitation.
5. the preparation method of the neutral bone cement of anti-collapsibility injectable according to claim 1, it is characterized in that, the manner of formulation of the consolidation liquid of the sodium carboxymethyl cellulose modification that step (2) is described is that room temperature is dissolved, or ultrasonic dissolution assisting, can also be aided with mechanical agitation or magnetic agitation.
6. the preparation method of the neutral bone cement of anti-collapsibility injectable according to claim 1, is characterized in that, the described pre-molten mode of step (3) is for 37 ℃ of mobility that add below the consolidation liquid of heat gain sodium carboxymethyl cellulose modification.
7. the preparation method of the neutral bone cement of anti-collapsibility injectable according to claim 1, 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 neutral bone cement of anti-collapsibility injectable preparing according to method described in claim 1-7 any one; Its pH value in water is 5-9, and defeated and dispersed coefficient is not more than 1%, and injectability coefficient is not less than 35%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN105999418A (en) * | 2016-06-20 | 2016-10-12 | 北京大学口腔医院 | Injectable bioactive bone cement material 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 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105999418A (en) * | 2016-06-20 | 2016-10-12 | 北京大学口腔医院 | Injectable bioactive bone cement material 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 |
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