CN103656753B - Neutral calcium phosphate bone cement and preparation method thereof - Google Patents
Neutral calcium phosphate bone cement and preparation method thereof Download PDFInfo
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- CN103656753B CN103656753B CN201310642406.5A CN201310642406A CN103656753B CN 103656753 B CN103656753 B CN 103656753B CN 201310642406 A CN201310642406 A CN 201310642406A CN 103656753 B CN103656753 B CN 103656753B
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Abstract
The invention relates to a method belonging to the technical field of biomedical materials, and concretely relates to a neutral calcium phosphate bone cement and a preparation method thereof. The preparation method is characterized in that the preparation method comprises the following steps: preparing a bone cement powder main component by appropriately controlling reaction conditions; adding a certain amount of hydroxyapatite and silicate to the above powder, and fully and uniformly mixing to prepare bone cement powder; and blending the bone cement powder with a citric acid-containing solidification liquid according to a certain liquid/solid ratio to obtain neutral bone cement, and putting solidified bone cement in water to obtain a neutral solution. The preparation method of the neutral bone cement enriches the range of the bone cement powder, allows acidic solidification liquids to be widely applied in injectable bone cements, and has the advantages of simplicity, feasibility, good effect, suitableness for the popularization in different acidic solidification liquids, and large scale application.
Description
Technical field
The present invention relates to a kind of method of biology medical material technical field, specifically a kind of neutral calcium phosphate pastern bone cement and preparation method thereof.
Background technology
In some calcium phosphate bone cement systems, in order to promote bone cement powder curing molding better and keep high compressive strength, general needs add a large amount of citric acids ［ M. Anirban Jyoti, Applied Surface Science, 2010 ］ in bone cement consolidation liquid.Blemish in an otherwise perfect thing, citric acid is effectively promoting bone cement curing molding and while keeping advantages of higher compressive strength, is also often causing bone cement to be highly acid.The existence of a large amount of proton generally can cause cell death, seriously limits its application in vivo.
The present invention is directed to above background with not enough, bone cement of a kind of novelty and preparation method thereof is provided, by regulating and controlling preparation technology and the composition of bone cement, while raising bone cement mechanical strength, the highly acid problem that can effectively avoid traditional method to bring.
Summary of the invention
Neutral bone cement that the object of the present invention is to provide a kind of novelty and preparation method thereof, be grouped into by the preparation technology and one-tenth thereof that regulate and control bone cement, while raising bone cement mechanical strength, the highly acid problem of the bone cement that can effectively avoid traditional method to bring.
Object of the present invention is achieved through the following technical solutions: fully mixed with calcium carbonate powder by a certain proportion of calcium hydrogen phosphate; Then adopting the method for solid state reaction, preparing bone cement powder bulk composition by controlling reaction condition rightly.A certain amount of hydroxyapatite is added on this basis and the abundant mix homogeneously of silicate prepares bone cement powder in powder.Bone cement powder is in harmonious proportion by certain liquid-solid ratio with containing the consolidation liquid of citric acid, hardening time can be obtained without significant prolongation or the neutral bone cement that shortens to some extent.
A preparation method for neutral calcium phosphate bone cement, is characterized in that, comprises the following steps:
(1) bone cement powder bulk composition is obtained after calcination in 900 DEG C of stoves after being mixed by raw material, ball milling;
(2) in bone cement powder bulk composition, hydroxyapatite is added and silicate prepares bone cement powder;
(3) if bone cement powder for a long time need not, be stored in 4 DEG C of dry enclosed environments;
(4) bone cement powder and acid consolidation liquid are in harmonious proportion by liquid-solid ratio, can neutral calcium phosphate bone cement be obtained.
Calcium hydrogen phosphate and the calcium carbonate mixture of to be mol ratio be 2:0.90 to the 2:1.15 of the raw material described in step (1).
Hydroxyapatite described in step (2) is of a size of and is less than 5 mm, and its content in bone cement powder is 0.05-60%.
Silicate described in step (2) is one in sodium silicate, potassium silicate, calcium silicates or its combination, and its content in bone cement is 0-30%.
Dry enclosed environment described in step (3) is that outside air can not directly contact with bone cement powder.
Dry enclosed environment described in step (3) for bone cement powder is placed in the inert gas environment such as nitrogen, argon, or is placed on after evacuation in exsiccator, electronic dry cabinet.
Acid consolidation liquid described in step (4) is the solution of citric acid content at 3-55%, or based on it, add 0.01-5% hydroxypropyl emthylcellulose, the sodium carboxymethyl cellulose of 0.01-2%, 0.01-4% chitosan, 0.01-2% gelatin, 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, 0.01-5% cyclodextrin one wherein or its combination.
Liquid-solid ratio described in step (4) is add 0.30-0.70 milliliter consolidation liquid in every 1 gram of bone cement powder.
The neutral calcium phosphate bone cement that method prepares according to above-mentioned any one, its pH value is 5-9, and after solidification, apparent density is not less than 1.30 g/cm
3, defeated and dispersed coefficient is not more than 5%.
The present invention is grouped into by the preparation technology and one-tenth thereof regulating and controlling bone cement and prepares a kind of Bone Colonizable Cements In Rabbits powder.Gained bone cement powder can effectively with citric acid system consolidation liquid curing molding, keep higher mechanical strength simultaneously.Preparation method provided by the invention is simple, easy, effective, be suitable for promoting the use of in the consolidation liquid system of difference containing citric acid, can large-scale application.
Apparent density method of testing is: first adopt the cylindrical mold of diameter 6 mm height 10 mm to prepare bone cement sample, then measure the actual diameter of the bone cement sample of solidification after 24 hours, height and quality, calculate its density and be apparent density.
The method of testing of defeated and dispersed coefficient is: after solidifying, bone cement to soak after 10 days Mass lost percentage ratio as defeated and dispersed coefficient in water.
PH value method of testing containing bone cement aqueous solution is: the bone cement after 1.0 g are solidified 24 hours is placed in 20 mL ultra-pure waters, then measures its pH value in different soak time with pH meter.
Accompanying drawing explanation
After Figure 1 shows that solidification, bone cement is placed on solution ph change curve in time after in water.
Detailed description of the invention
Following examples are implemented premised on invention technical scheme, give 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 DEG C of vacuum drying ovens, drying obtains mixed powder.After 900 DEG C of stove stage casings burn 15 hours, wet ball grinding is adopted to obtain bone cement dispersion liquid powder body.Obtain bone cement powder bulk composition after dispersion liquid is centrifugal, drying, powder body is of a size of 300-800 nm.
Embodiment 2:
96 g bone cement powder bulk composition and 4 g hydroxyapatite mortar grinder are evenly obtained bone cement powder.The consolidation liquid of 20% citric acid-1% hydroxypropyl emthylcellulose composition and bone cement powder are in harmonious proportion by the liquid-solid ratio of 0.5 mL/g, it is 11 min that reference standard ASTM C191 measures the presetting period.After solidification, bone cement apparent density is 1.45 g/cm
3, defeated and dispersed coefficient is 1.5%.Be added to the water, solution is in neutral.After leaving standstill one week, test solution pH is substantially constant, and as shown in Figure 1, aqueous solution pH keeps neutral at long period yardstick always.
Embodiment 3:
91 g bone cement powder bulk composition and 4 g hydroxyapatite and 5 g sodium silicate mortar grinder are evenly obtained bone cement powder.The consolidation liquid of 20% citric acid-1% hydroxypropyl emthylcellulose composition and bone cement powder are in harmonious proportion by the liquid-solid ratio of 0.5 mL/g, it is 9 min that reference standard ASTM C191 measures the presetting period.After solidification, bone cement apparent density is 1.48 g/cm
3, defeated and dispersed coefficient 2.2%.Be added to the water, solution is in neutral.After leaving standstill one week, pH value of solution is substantially constant, similar shown in result and Fig. 1.
Claims (4)
1. a preparation method for neutral calcium phosphate bone cement, is characterized in that, comprises the following steps:
(1) bone cement powder bulk composition is obtained after calcination in 900 DEG C of stoves after being mixed by raw material, ball milling;
Calcium hydrogen phosphate and the calcium carbonate mixture of described raw material to be mol ratio be 2:0.90 to 2:1.15;
(2) in bone cement powder bulk composition, hydroxyapatite is added and silicate prepares bone cement powder;
Described hydroxyapatite is of a size of and is less than 5 mm, and its content in bone cement powder is 0.05-60%;
Described silicate is one in sodium silicate, potassium silicate, calcium silicates or its combination, and its content in bone cement is 0-30%;
(3) if bone cement powder for a long time need not, be stored in 4 DEG C of dry enclosed environments;
(4) bone cement powder and acid consolidation liquid are in harmonious proportion by liquid-solid ratio, can neutral calcium phosphate bone cement be obtained;
Described acid consolidation liquid is the solution of citric acid content at 3-55%, or based on it, add 0.01-5% hydroxypropyl emthylcellulose, the sodium carboxymethyl cellulose of 0.01-2%, 0.01-4% chitosan, 0.01-2% gelatin, 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, 0.01-5% cyclodextrin one wherein or its combination, described liquid-solid ratio is add 0.30-0.70 milliliter consolidation liquid in every 1 gram of bone cement powder.
2. the preparation method of neutral calcium phosphate bone cement according to claim 1, it is characterized in that, the dry enclosed environment described in step (3) is that outside air can not directly contact with bone cement powder.
3. the preparation method of neutral calcium phosphate bone cement according to claim 2, it is characterized in that, dry enclosed environment described in step (3) for bone cement powder is placed in nitrogen, argon inert gas environment, or is placed on after evacuation in exsiccator, electronic dry cabinet.
4. the neutral calcium phosphate bone cement that method prepares according to claim 1-3 any one, its pH value is 5-9, and after solidification, apparent density is not less than 1.30 g/cm
3, defeated and dispersed coefficient is not more than 5%.
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| CN104524627B (en) * | 2014-12-23 | 2016-08-17 | 南京航空航天大学 | The preparation method of the hydroxyapatite bone cement of high intensity |
| CN106267365A (en) * | 2016-08-17 | 2017-01-04 | 林春梅 | A kind of enhancing activity injecting bone cement and preparation method thereof |
| CN106729971B (en) * | 2016-11-23 | 2019-12-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Water-soluble single-walled carbon nanotube modified calcium phosphate cement and preparation and application thereof |
| CN106540317A (en) * | 2016-12-08 | 2017-03-29 | 苏州艾博迈尔新材料有限公司 | A kind of realizing controlled-release bone cement and preparation method thereof |
| CN106620886A (en) * | 2016-12-09 | 2017-05-10 | 苏州纳贝通环境科技有限公司 | Liquid bracket material for bone repair and preparation method thereof |
| CN108273131B (en) * | 2018-03-19 | 2021-07-27 | 深圳市中科海世御生物科技有限公司 | Composite bone cement, preparation method and application thereof, and bone repair material |
| CN109498846B (en) * | 2018-10-09 | 2021-07-16 | 广州润虹医药科技股份有限公司 | Bone repair scaffold capable of releasing zinc ions and strontium ions simultaneously and preparation method thereof |
| CN110201228A (en) * | 2019-04-19 | 2019-09-06 | 湖北联结生物材料有限公司 | A kind of calcium phosphate bone cement and its preparation method and application containing decalcified bone matrix |
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