WO2019148554A1 - 一种硼磷系生物活性玻璃及其制备方法 - Google Patents
一种硼磷系生物活性玻璃及其制备方法 Download PDFInfo
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- WO2019148554A1 WO2019148554A1 PCT/CN2018/077009 CN2018077009W WO2019148554A1 WO 2019148554 A1 WO2019148554 A1 WO 2019148554A1 CN 2018077009 W CN2018077009 W CN 2018077009W WO 2019148554 A1 WO2019148554 A1 WO 2019148554A1
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- WIPO (PCT)
- Prior art keywords
- boron
- glass
- preparing
- phosphorus
- bioactive glass
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/14—Silica-free oxide glass compositions containing boron
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/18—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/10—Ceramics or glasses
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/54—Biologically active materials, e.g. therapeutic substances
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/58—Materials at least partially resorbable by the body
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/0007—Compositions for glass with special properties for biologically-compatible glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/0007—Compositions for glass with special properties for biologically-compatible glass
- C03C4/0014—Biodegradable glass
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/112—Phosphorus-containing compounds, e.g. phosphates, phosphonates
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/412—Tissue-regenerating or healing or proliferative agents
Definitions
- the invention belongs to the field of biomedical technology, and in particular relates to a bioactive glass for surface tissue damage repair and a preparation method thereof.
- the object of the present invention is to prepare a core-shell structured borophosphate bioactive glass by a simple impregnation method to obtain excellent tissue repair ability and biocompatibility.
- the present invention is implemented by the following technical solutions:
- a boron-phosphorus bioactive glass and a preparation method thereof the selected initial glass is a boron-based glass, and the raw material composition is B 2 O 3 , MgO, CaO, Na 2 O, K 2 O and SrO, and the mass ratio thereof is 45 ⁇ 60:2 ⁇ 10:15 ⁇ 25:3 ⁇ 10:10 ⁇ 15:1 ⁇ 8.
- the initial glass is obtained by high-temperature melt cooling to obtain a glass frit, which is sieved to obtain a glass powder.
- the melting temperature is 1000-1350 ° C
- the holding time is 0.5-4 hours, preferably 1100-1300 ° C
- the temperature is 0.5-2 hours.
- the experimental instruments used in the method such as a beaker, a stir bar, a measuring cylinder, etc., are washed with ultrapure water and subjected to sterilization and sterilization;
- the raw materials required for the impregnation solution are arranged according to the ratio, and are stirred and dissolved for use; the components of the impregnated solution are CaCl 2 , (NH 4 ) 2 HPO 4 , K 2 HPO 4 ⁇ 3H 2 O, HCl, dissolved in 1 L.
- the mass ratio is 5 ⁇ 20:15 ⁇ 25:60 ⁇ 70:0.1 ⁇ 2; the CaCl 2 , (NH 4 ) 2 HPO 4 , K 2 HPO 4 ⁇ 3H 2 O are analyzed. Pure, HCl concentration is 0.1mol / L;
- a medical solvent is added to the glass frit to prepare a bioglass coating material.
- the appliance is disinfected and sterilized, and the operator and the environment are also required to maintain a high degree of sterility to ensure that no harmful substances are introduced during the experiment;
- the grinding medium used for the polishing of the bioglass is an agate mortar;
- the sieve used is a food grade stainless steel sieve, the sieve is a 325 mesh, 270 mesh sieve, and the intermediate layer glass powder is used after sieving. .
- the main purpose of the hydrochloric acid used is to adjust the pH value of the solution, and after the solution is prepared, the pH of the solution is weakly acidic.
- step (4) it is necessary to confirm the uniform dispersion of the glass powder during the stirring process, and there is no agglomeration or agglomerate to ensure sufficient contact between the glass powder and the immersion liquid.
- vacuum filtration uses a filter paper having a pore diameter of less than 30 ⁇ m to control the dropping rate and the degree of vacuum of the solution to prevent pore clogging and damage of the filter paper.
- the ultrapure water washing is carried out for 3 cycles to ensure that the glass powder is cleaned comprehensively.
- the medical solvent used in the step (7) is a mixture of liquid paraffin, polyethylene glycol, carboxymethyl chitosan, sodium hyaluronate or the like;
- the steps (1) to (7) need to be carried out in a biomedical laboratory with high cleanliness to ensure the accuracy of the experimental process.
- the porous phosphate shell can not only control the degradation rate of the borate glass structure in the living body, but also improve the biocompatibility of the biomaterial and significantly improve the repair speed of the damaged surface tissue;
- the raw material of the invention is simple and easy to obtain, the preparation method is simple, the process is stable, and the conditions of practicalization and industrialization are achieved.
- Figure 1 shows the wound healing of a control sample
- Figure 2 is a view of wound healing after use of borophosphorus glass
- Figure 3 is a comparison of in vitro cell culture of the respective examples.
- a boron-phosphorus bioactive glass and a preparation method thereof the initial bioglass selected is boron-based glass, and the raw material composition is B 2 O 3 , MgO, CaO, Na 2 O, K 2 O and SrO, and the mass ratio thereof is 45 ⁇ 60:2 ⁇ 10:15 ⁇ 25:3 ⁇ 10:10 ⁇ 15:1 ⁇ 8.
- the initial glass has a melting temperature of 1000 to 1350 ° C, a holding time of 0.5 to 4 hours, preferably 1100 to 1300 ° C, and a holding temperature of 0.5 to 2 hours.
- the impregnated solution components are CaCl 2 , (NH 4 ) 2 HPO 4 , K 2 HPO 4 ⁇ 3H 2 O, HCl, dissolved in 1 L of ultrapure water, and the mass ratio is 5-20:15 ⁇ 25:60 ⁇ 70: 0.1 ⁇ 2.
- the specific steps are as follows:
- the experimental instruments used in the method such as a beaker, a stir bar, a measuring cylinder, etc., are washed with ultrapure water and subjected to sterilization and sterilization;
- a medical solvent is added to the glass frit to prepare a bioglass coating material.
- the appliance is disinfected and sterilized, and the operator and the environment are also required to maintain a high degree of sterility to ensure that no harmful substances are introduced during the experiment;
- the grinding medium used for the polishing of the bioglass is an agate mortar;
- the sieve used is a food grade stainless steel sieve, the sieve is a 325 mesh, 270 mesh sieve, and the intermediate layer glass powder is used after sieving. .
- the main purpose of the hydrochloric acid used is to adjust the pH value of the solution, and after the solution is prepared, the pH of the solution is weakly acidic.
- step (4) it is necessary to confirm the uniform dispersion of the glass powder during the stirring process, and there is no agglomeration or agglomerate to ensure sufficient contact between the glass powder and the immersion liquid.
- vacuum filtration uses a filter paper having a pore diameter of less than 30 ⁇ m to control the dropping rate and the degree of vacuum of the solution to prevent pore clogging and damage of the filter paper.
- the ultrapure water washing is carried out for 3 cycles to ensure that the glass powder is cleaned comprehensively.
- the medical solvent used in the step (7) is a mixture of liquid paraffin, polyethylene glycol, carboxymethyl chitosan, sodium hyaluronate or the like;
- the steps (1) to (7) need to be carried out in a biomedical laboratory with high cleanliness to ensure the accuracy of the experimental process.
- Table 1 is a table of initial glass components (in mass percent) in Examples 1-4
- each component in Table 1 weigh a certain amount of analytically pure raw materials (B 2 O 3 , MgO, CaO, Na 2 O, K 2 O and SrO), mix them evenly and put the powder into platinum. It is placed in a box-type resistance furnace for melting (melting temperature is 1350 ° C, holding time is 2 hours). The melt is then poured into deionized water to be quenched, dried to obtain a glass frit, and after ball milling, a glass frit is obtained. A certain amount of CaCl 2 , (NH 4 ) 2 HPO 4 , K 2 HPO 4 ⁇ 3H 2 O, HCl (mass ratio: 5:23:70:2) was weighed and dissolved in 1 L of ultrapure water.
- analytically pure raw materials B 2 O 3 , MgO, CaO, Na 2 O, K 2 O and SrO
- each component in Table 1 weigh a certain amount of analytically pure raw materials (B 2 O 3 , MgO, CaO, Na 2 O, K 2 O and SrO), mix them evenly and put the powder into platinum. It is placed in a box-type resistance furnace for melting (melting temperature is 1300 ° C, holding time is 2 hours). The melt is then poured into deionized water to be quenched, dried to obtain a glass frit, and after ball milling, a glass frit is obtained.
- analytically pure raw materials B 2 O 3 , MgO, CaO, Na 2 O, K 2 O and SrO
- each component in Table 1 weigh a certain amount of analytically pure raw materials (B 2 O 3 , MgO, CaO, Na 2 O, K 2 O and SrO), mix them evenly and put the powder into platinum. It is placed in a box-type resistance furnace for melting (melting temperature is 1200 ° C, holding time is 2 hours). The melt is then poured into deionized water to be quenched, dried to obtain a glass frit, and after ball milling, a glass frit is obtained. A certain amount of CaCl 2 , (NH 4 ) 2 HPO 4 , K 2 HPO 4 ⁇ 3H 2 O, HCl (mass ratio: 15:15:69:1) was weighed and dissolved in 1 L of ultrapure water.
- analytically pure raw materials B 2 O 3 , MgO, CaO, Na 2 O, K 2 O and SrO
- FIGS. 1 to 2 are graphs of wound healing of the control sample glass and Example 3, and it can be seen from the figure that Example 3 can effectively promote wound healing.
- each component in Table 1 weigh a certain amount of analytically pure raw materials (B 2 O 3 , MgO, CaO, Na 2 O, K 2 O and SrO), mix them evenly and put the powder into platinum. It is placed in a box-type resistance furnace for melting (melting temperature is 1100 ° C, holding time is 2 hours). The melt is then poured into deionized water to be quenched, dried to obtain a glass frit, and after ball milling, a glass frit is obtained.
- analytically pure raw materials B 2 O 3 , MgO, CaO, Na 2 O, K 2 O and SrO
- the present invention realizes a boron phosphorus bioactive glass and a preparation method thereof by the above embodiments. Its remarkable effects are concentrated in excellent biocompatibility and ability to promote tissue repair.
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Abstract
Description
Claims (10)
- 一种硼磷系生物活性玻璃的制备方法,其特征在于:通过熔融冷却法制备硼系玻璃,其原料组成为B 2O 3、MgO、CaO、Na 2O、K 2O和SrO,然后通过含磷离子的浸渍溶液进行浸渍,获得多孔的磷酸盐为外壳,硼酸盐为内核的双层生物活性玻璃。
- 根据权利要求1所述的一种硼磷系生物活性玻璃的制备方法,其特征在于:所述硼系玻璃,其原料组成为B 2O 3、MgO、CaO、Na 2O、K 2O和SrO,其质量比为45~60:2~10:15~25:3~10:10~15:1~8。
- 根据权利要求2所述的一种硼磷系生物活性玻璃的制备方法,其特征在于:所述硼系玻璃,其原料组成为B 2O 3、MgO、CaO、Na 2O、K 2O和SrO,其质量比为50~58:3~8:15~20:3~10:10~15:2~7。
- 根据权利要求1所述的一种硼磷系生物活性玻璃的制备方法,其特征在于:所述浸渍溶液成分为CaCl 2、(NH 4) 2HPO 4、K 2HPO 4×3H 2O、HCl,其质量比为5~20:15~25:60~70:0.1~2,溶解在1L的超纯水中。
- 根据权利要求1所述的一种硼磷系生物活性玻璃的制备方法,其特征在于:具体操作步骤如下:(1)对所需的实验器具,如烧杯、搅拌棒、量筒用超纯水清洗,并进行消毒杀菌处理;(2)采用熔融冷却的方法制得硼系初始玻璃熔块,将硼系玻璃磨碎过筛,获得粒径30~45μm玻璃粉,并对玻璃粉进行消毒杀菌处理;(3)将浸渍溶液所需原料按照配比配置,搅拌溶解后备用;(4)称取100 g玻璃粉末,放入1L浸渍溶液中,持续搅拌1~8h;(5)采用真空过滤法将浸渍后的玻璃粉进行固液分离;(6)将分离后的玻璃粉用超纯水在真空过滤装置中进行清洗,烘干后备用;(7)在处理后的硼系玻璃粉中加入医用溶剂,制备成生物玻璃涂敷料。
- 根据权利要求5所述的一种硼磷系生物活性玻璃的制备方法,其特征在于:步骤(2)所述硼系初始玻璃的熔制温度为1000-1350℃,保温时间为0.5~4小时。
- 根据权利要求6所述的一种硼磷系生物活性玻璃的制备方法,其特征在于:熔制温度为1100-1300℃,保温0.5-2小时。
- 根据权利要求5所述的一种硼磷系生物活性玻璃的制备方法,其特征在于:步骤(4)所述持续搅拌时间为3-6h。
- 根据权利要求5所述的一种硼磷系生物活性玻璃的制备方法,其特征在于:所述步骤(7)中所使用的医用溶剂为液体石蜡、聚乙二醇、羧甲基壳聚糖、透明质酸钠的混合物。
- 一种如权利要求1所述方法制备的硼磷系生物活性玻璃。
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CN113165951A (zh) * | 2018-09-05 | 2021-07-23 | 艾尔科学股份有限公司 | 玻璃组合物 |
CN109437559B (zh) * | 2018-11-19 | 2021-09-14 | 湖北中创医疗用品有限公司 | 生物活性玻璃、生物活性玻璃凝胶及其制备方法和应用 |
CN109985272B (zh) * | 2019-03-07 | 2022-05-13 | 中国科学院合肥物质科学研究院 | 硼磷酸盐生物玻璃复合材料及其制备方法和用途 |
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US6709744B1 (en) * | 2001-08-13 | 2004-03-23 | The Curators Of The University Of Missouri | Bioactive materials |
CN102430149A (zh) * | 2011-11-18 | 2012-05-02 | 华东理工大学 | 一种硼磷酸盐玻璃纤维/壳聚糖复合材料 |
WO2014159240A1 (en) * | 2013-03-14 | 2014-10-02 | Novabone Products, Llc | Compositions and methods for manufacturing sol-gel derived bioactive borophosphate glasses for medical applicatons |
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CN107617121A (zh) * | 2017-10-13 | 2018-01-23 | 广州润虹医药科技股份有限公司 | 一种皮肤创面生物诱导活性敷料及其制备方法和应用 |
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CN102430149A (zh) * | 2011-11-18 | 2012-05-02 | 华东理工大学 | 一种硼磷酸盐玻璃纤维/壳聚糖复合材料 |
WO2014159240A1 (en) * | 2013-03-14 | 2014-10-02 | Novabone Products, Llc | Compositions and methods for manufacturing sol-gel derived bioactive borophosphate glasses for medical applicatons |
CN106630646A (zh) * | 2016-12-09 | 2017-05-10 | 苏州纳贝通环境科技有限公司 | 一种多孔生物玻璃陶瓷及其制备方法 |
CN107617121A (zh) * | 2017-10-13 | 2018-01-23 | 广州润虹医药科技股份有限公司 | 一种皮肤创面生物诱导活性敷料及其制备方法和应用 |
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