CN103977454A - Magnesium phosphate/wheat protein composite material, as well as preparation method and application thereof - Google Patents
Magnesium phosphate/wheat protein composite material, as well as preparation method and application thereof Download PDFInfo
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- CN103977454A CN103977454A CN201410231324.6A CN201410231324A CN103977454A CN 103977454 A CN103977454 A CN 103977454A CN 201410231324 A CN201410231324 A CN 201410231324A CN 103977454 A CN103977454 A CN 103977454A
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Abstract
The invention discloses a magnesium phosphate/wheat protein composite material, as well as a preparation method and application thereof. The preparation method of the magnesium phosphate/wheat protein composite material comprises the following steps: mixing magnesium phosphate and wheat protein in a mass ratio of 1:4-2:3, and performing ball milling and compression molding. The magnesium phosphate/wheat protein composite material has excellent biocompatibility, has the degradation rate matched with new bone growth and has an excellent bone repairing ability, the raw material source is wide, the degraded system environment is suitable for bone cell growth, and the composite material can be used as a bone regeneration scaffold. The preparation method of the magnesium phosphate/wheat protein composite material is easy to operate, and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of magnesium phosphate/wheat protein composite and its preparation method and application.
Background technology
Artificial bone repair materials can be divided into again organic material, the large class of inorganic material two; Organic material is as collagen, polylactic acid, chitosan, polycaprolactone etc.; Inorganic material comprises hydroxyapatite, calcium phosphate, magnesium phosphate, bioactivity glass, calcium sulfate etc.These artificial bone repair materials are widely used in Tissue Engineering Study, but also expose some defects and deficiency in application process, mechanical strength as common in organic material is not good enough, hydrophilic also or short ability of cell proliferation not good enough; And inorganic material is as excessive in bio-vitric, bioceramic much higher hard, fragility, its degradation rate of the bone alternate materials such as calcium phosphate, calcium sulfate does not mate with new bone growth.
Magnesium elements is one of skeletogenous necessary mineral of group, accounts for the 0.5%-1% of skeleton total mineral content, and metabolism and growth to skeleton play an important role.In recent years, mg-based material becomes a focus of biomedical sector as the research of bone renovating material.The research of mg-based material is mainly comprised to the following aspects: magnesium and alloy thereof, containing magnesium bio-vitric, containing magnesium bioceramic, containing magnesium biological bone cement with containing magnesium biological coating etc.Have scientific research personnel to prepare artificial bone graft's material with half-H 2 O calcium sulphate and magnesium phosphate, but this material is larger on system pH impact in degradation process, has reached 9.0, this alkaline environment is unfavorable for the growth of cell.Also have about fibroin albumen/calcium phosphate composite material, the correlational study of aminoacid/calcium phosphate composite material, but in article, only carried out experiment in vitro, its bone repairing effect is in animal body still unknown.
At present, it is animal proteinum (as collagen etc.) that tissue renovation material is studied more protide biomaterial, but animal proteinum extraction process bothers, and price is more expensive, and may have potential safety hazard, such as immunological rejection and source of disease propagation etc.Vegetable protein (as zein, wheat protein etc.) is to extract from plant, and it is compared with animal proteinum, and wide material sources, cheap and easy to get, easy to make, are suitable for being widely used in biomedical sector.Have been reported in the world the research of a vegetable protein (zein) as drug release carrier and tissue engineering material.Wheat protein has good degradability and biocompatibility, and wheat protein is made liver-targeted nanometer compositions by existing scientific research personnel, or by itself and the compound capsule for the preparation of drug delivery of polylactic acid, or use it for and prepare medical films etc.
Summary of the invention
The invention solves bone renovating material in prior art does not mate with new bone growth, after its degraded, system environment is unsuitable for undesirable etc. the defect of the increment of osteocyte and differentiation, skeletonization amount, and a kind of magnesium phosphate/wheat protein composite and its preparation method and application is provided.Magnesium phosphate/wheat protein composite of the present invention has good biocompatibility, its degradation rate and new bone growth match, and have good bone repair ability, and its raw material sources are extensive, system environment after degraded is suitable for bone cell growth, can be used as osteanagenesis support.The preparation method of magnesium phosphate/wheat protein composite of the present invention is simple to operate, is suitable for suitability for industrialized production.
The present invention solves the problems of the technologies described above by the following technical programs.
The invention provides a kind of preparation method of magnesium phosphate/wheat protein composite, it comprises the steps: magnesium phosphate and wheat protein to mix with the mass ratio of 1:4～2:3, ball milling, and compression molding, to obtain final product.
Wherein, described magnesium phosphate is the conventional magnesium phosphate using in this area, and its particle diameter is generally 400-700nm.
Wherein, described wheat protein is the conventional wheat protein using in this area.
Wherein, the method for described ball milling and condition can be method and the condition of this area routine.The rotating speed of described ball milling is preferably 150-250r/min.The ratio of grinding media to material of described ball milling is preferably 1.2:1-1.8:1.The time of described ball milling is preferably 10-14 hour.
Wherein, the method for described compression molding and condition can be method and the condition of this area routine.The pressure of described compression molding is preferably 1.5-2.5MPa.The dwell pressure of described compression molding is preferably 2-3 minute.The mould of described compression molding is preferably stainless steel mould.According to this area general knowledge, the large I of the specification of described stainless steel mould is adjusted according to actual needs.
It is a kind of by the prepared magnesium phosphate/wheat protein of above-mentioned preparation method composite that the present invention also provides.
The present invention also provides the application of described magnesium phosphate/wheat protein composite in osteanagenesis support.
Meeting on the basis of this area general knowledge, above-mentioned each optimum condition, can combination in any, obtains the preferred embodiments of the invention.
Agents useful for same of the present invention and raw material be commercially available obtaining all.
Positive progressive effect of the present invention is:
Magnesium phosphate/wheat protein composite of the present invention has good biocompatibility, and after it dissolves in Tris-HCl solution, the pH environment forming is applicable to the growth of osteocyte very much.This magnesium phosphate/wheat protein composite also has good histocompatibility, and degradability and osteoinductive have good bone reparation property, can be used as osteanagenesis support.
Brief description of the drawings
Fig. 1 is the stereoscan photograph of wheat protein, embodiment 1 and 2 samples.
Fig. 2 is the weight-loss ratio variation diagram after wheat protein, embodiment 1 and 2 samples are immersed in Tris-HCl solution.
Fig. 3 is after wheat protein, embodiment 1 and 2 samples are immersed in Tris-HCl solution, the pH value variation diagram of solution.
Fig. 4 Fig. 3 is that wheat protein, embodiment 1 and 2 samples were immersed in SBF simulated body fluid after 7 days, the stereoscan photograph of sample.
Fig. 5 is embodiment 2 samples Sr-X radiographs 4,8 and 12 weeks time behind the damaged place of implantable bone.
Fig. 6 is the embodiment 2 samples dyeing of the HE 4,8 and 12 weeks time tissue slice figure behind the damaged place of implantable bone.
Detailed description of the invention
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, according to conventional method and condition, or selects according to catalogue.
In following embodiment, magnesium phosphate used is purchased from Chemical Reagent Co., Ltd., Sinopharm Group, and its particle diameter is 400-700nm; Wheat protein used is purchased from changing into Co., Ltd. in Tokyo.
Embodiment 1
A kind of preparation method of magnesium phosphate/wheat protein composite, it comprises the steps: magnesium phosphate and wheat protein to mix with the mass ratio of 1:4, with the rotating speed ball milling of 150r/min 10 hours, wherein ratio of grinding media to material is 1.2:1, then by material after ball milling under the pressure of 2.5MPa, in stainless steel mould, carry out compression molding, the dwell time is 2min, to obtain final product.
Embodiment 2
A kind of preparation method of magnesium phosphate/wheat protein composite, it comprises the steps: magnesium phosphate and wheat protein to mix with the mass ratio of 2:3, with the rotating speed ball milling of 250r/min 14 hours, wherein ratio of grinding media to material is 1.8:1, then by material after ball milling under the pressure of 1.5MPa, in stainless steel mould, carry out compression molding, the dwell time is 3min, to obtain final product.
Effect embodiment
(1) sample surface morphology
According to the compression molding condition in embodiment 1, wheat protein is carried out to tabletting (specification is Φ 12 × 2mm).Magnesium phosphate/wheat protein composite that wheat protein, embodiment 1 and 2 are obtained carries out scanning electron microscope (JEOL-6360LV, Japan) test, to observe the surface topography of sample, result as shown in Figure 1, wherein figure (a), (b) and (c) be respectively the SEM photo of wheat protein, embodiment 1 and embodiment 2 samples.As can be seen from Figure 1, the smooth surface of wheat protein disk is smooth, and the sample surfaces of embodiment 1 and 2 is coarse, dispersed some white granules.
(2) external degradation performance test
Magnesium phosphate/wheat protein composite that embodiment 1 and 2 is obtained carries out external degradation performance test.The initial mass of testing sample (specification is Φ 12 × 2mm) is W
0, testing sample is joined in Tris-HCl buffer according to the ratio of 0.1g/20mL, in the constant temperature oscillation case of 37 DEG C, cultivate with the frequency oscillation of 120rpm, changed a not good liquor every 3 days.Sampling in the time of 3,7,14,21,28,42 and 49 days, after cleaning, is dried to constant weight with distilled water, weighs sample quality Wt.Degradation rate represents with different time points weight-loss ratio, calculates with following formula: weight-loss ratio (%)=[(W
0-W
t)/W
0] × 100%.Test result as shown in Figure 2.In addition, measure respectively the pH value of Tris-HCl buffer in experimentation at 0,12,24,72,120,168 and 300 hour with pH meter, test result is shown in Fig. 3.
As can be seen from Figure 2, the 49th day time, the weight-loss ratio of wheat protein sample, embodiment 1 and embodiment 2 is respectively 51.53%, 49.38%, 37.64%, and the degradation rate of magnesium phosphate/wheat protein composite is slow compared with wheat protein disk, and its weight-loss ratio after 42 days remains unchanged substantially.As can be seen from Figure 3, magnesium phosphate/wheat protein composite is in degradation process, and the pH value of solution slightly raises, but finally maintains stable pH value level; And wheat protein sample is in degradation process, there is slight decline in the pH value of solution.To recently seeing, the subalkaline environment that magnesium phosphate/wheat protein composite forms in degradation process, is more conducive to increment and the differentiation of osteocyte.
In addition magnesium phosphate/wheat protein the composite, wheat protein, embodiment 1 and 2 being obtained carries out immersion test in SBF simulated body fluid.In the constant-temperature table of 37 DEG C, carry out this immersion test, soak sampling afterwards in 7 days, carefully clean sample and dry with deionized water.The sample of wheat protein, embodiment 1 and 2 is soaking SEM photo after 7 days respectively as Fig. 4 (a), (b) with (c).XRD and EDS test result from Fig. 4 in conjunction with each sample, in the immersion sample of wheat protein, be substantially devoid of apatite, in the immersion sample of embodiment 1 and 2, generate spherical apatite, and those apatite that are formed on composite material surface are not easy to come off, this shows that magnesium phosphate/wheat protein composite of the present invention has excellent Bioactivity, is suitable as bone renovating material.Wherein, Mg, P and the Ca content in each sample before and after soaking being obtained by EDS test is as shown in table 1.
Mg, P and the Ca content of table 1 in the each sample before and after SBF simulated body fluid immersion test
As can be seen from Table 1, the sample of embodiment 1 and 2 is after SBF simulated body fluid immersion test, Ca content wherein obviously increases, wheat protein sample is substantially devoid of Ca, this shows that magnesium phosphate/wheat protein composite of the present invention can induce the generation of apatite well, has bone inductive effect.
(3) animal is implanted experiment
The right femur joint defect of magnesium phosphate/wheat protein composite of embodiment 2 being implanted to New Zealand white rabbit, sample is process radiation sterilization before implantation.Fig. 5 (a), (b) and (c) be respectively implant after the Sr-X mating plate photo of gained 4,8 and 12 weeks time.As can be seen from the figure, composite implant is interior after 4 weeks, can obviously see the existence that bone is damaged, composite has started degraded, interface between sample and osseous tissue has had osseous tissue to start to grow into material internal, but the damaged sign of also not observing obvious healing of cortical bone now; After 8 weeks, along with growing into of osseous tissue, material is constantly degraded, and now damaged beginning of cortical bone heals; After 12 weeks, material is substantially degradable, and cortical bone defect is obviously healing.Visible, to bone, reparation has obvious facilitation to magnesium phosphate/wheat protein composite.
Fig. 6 (a), (b) and (c) HE that the freshman bone tissue when respectively to 4,8 and 12 weeks the carries out tissue slice figure that dyes, in figure, the B of labelling represents bone, M represents magnesium phosphate/wheat protein composite, and S represents bone marrow.As can be seen from Figure 6, composite implant is interior after 4 weeks, can see between material and osseous tissue, there is a very significantly interface by trichrome staining gained tissue slice, and around interface, there is the freshman bone tissue of many bluenesss, illustrate that osseous tissue starts to Material growth, also can find out same result by another colouring method HE dyeing; Implant after 8 weeks, composite is further degraded, and the interface between material and osseous tissue thickens, and freshman bone tissue further increases; Implant after 12 weeks, the osseous tissue that composite is connected to each other gradually replaces, and bone trabecula has run through bone defective region, and freshman bone tissue changes to ripe bone gradually, and defect heals substantially completely.
And the skeletonization amount data that draw by statistical analysis show, composite was implanted after 4 weeks, and defect skeletonization amount only has 15% left and right, and material starts degraded gradually, and 60% material remains in defect in addition; During by 8 weeks, skeletonization amount has approached 60%, and the remaining rate of composite probably has 40%; Implant after 12 weeks, skeletonization amount is up to 79%, and composite is substantially degradable, and defect has not substantially had composite.This explanation is along with the continuous degraded of magnesium phosphate/wheat protein composite, freshman bone tissue constantly generates, effectively repair defect, illustrate that magnesium phosphate/wheat protein composite has good bone reparation property, and can be in 12 weeks basic repair deficiency, this bone is repaired speed can mate bone formation rate well.
Claims (10)
1. a preparation method for magnesium phosphate/wheat protein composite, is characterized in that, it comprises the steps: magnesium phosphate and wheat protein to mix with the mass ratio of 1:4～2:3, ball milling, and compression molding, to obtain final product.
2. preparation method as claimed in claim 1, is characterized in that, the particle diameter of described magnesium phosphate is 400-700nm.
3. preparation method as claimed in claim 1 or 2, is characterized in that, the rotating speed of described ball milling is 150-250r/min.
4. preparation method as claimed in claim 1 or 2, is characterized in that, the ratio of grinding media to material of described ball milling is 1.2:1-1.8:1.
5. preparation method as claimed in claim 1 or 2, is characterized in that, the time of described ball milling is 10-14 hour.
6. preparation method as claimed in claim 1 or 2, is characterized in that, the pressure of described compression molding is 1.5-2.5MPa.
7. preparation method as claimed in claim 1 or 2, is characterized in that, the dwell pressure of described compression molding is 2-3 minute.
8. preparation method as claimed in claim 1 or 2, is characterized in that, the mould of described compression molding is stainless steel mould.
9. the prepared magnesium phosphate/wheat protein of a preparation method composite as described in claim 1-8 any one.
10. the application of magnesium phosphate/wheat protein composite as claimed in claim 9 in osteanagenesis support.
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Cited By (2)
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| CN107412879A (en) * | 2017-08-03 | 2017-12-01 | 上海蕴邦生物科技有限公司 | 3D printing compound rest and its preparation method and application |
| CN107412856A (en) * | 2017-08-03 | 2017-12-01 | 上海长海医院 | Nano-pore magnesium silicate microballoon/poly butylene succinate compound rest, protein coating compound rest and preparation method and application |
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| WO2008097529A1 (en) * | 2007-02-06 | 2008-08-14 | Dermal-Z Ltd. | Tissue compatible material and methods using same |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107412879A (en) * | 2017-08-03 | 2017-12-01 | 上海蕴邦生物科技有限公司 | 3D printing compound rest and its preparation method and application |
| CN107412856A (en) * | 2017-08-03 | 2017-12-01 | 上海长海医院 | Nano-pore magnesium silicate microballoon/poly butylene succinate compound rest, protein coating compound rest and preparation method and application |
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Inventor after: Wei Jie Inventor after: Kong Yao Inventor after: Xu Yiqiang Inventor after: Wang Quanxiang Inventor after: Ding Yueting Inventor after: Tang Xiaofeng Inventor after: Wu Yingyang Inventor after: Chen Jie Inventor after: Liu Changsheng Inventor after: Chen Xinju Inventor after: Liu Zhenghui Inventor before: Wei Jie Inventor before: Wang Quanxiang Inventor before: Liu Changsheng Inventor before: Tang Xiaofeng Inventor before: Chen Xinju Inventor before: Liu Zhenghui Inventor before: Kong Yao Inventor before: Xu Yiqiang |
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Free format text: CORRECT: INVENTOR; FROM: WEI JIE WANG QUANXIANG LIU CHANGSHENG TANG XIAOFENG CHEN XINJU LIU ZHENGHUI KONG YAO XU YIQIANG TO: WEI JIE WANG QUANXIANG DING YUETING TANG XIAOFENG WU YINGYANG CHEN JIE LIU CHANGSHENG CHEN XINJU LIU ZHENGHUI KONG YAO XU YIQIANG |
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Application publication date: 20140813 |