CN114668892A - 一种“鸡尾酒”型成骨抗菌型骨粉及其制备方法 - Google Patents
一种“鸡尾酒”型成骨抗菌型骨粉及其制备方法 Download PDFInfo
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Abstract
本发明涉及牙科植入材料加工与制备技术领域，尤其涉及一种“鸡尾酒”型成骨抗菌型骨粉及其制备方法，其组分按重量份计包括：羟基磷灰石粉30‑50份、聚甲基丙烯酸甲酯5‑10份、镁基金属微粉3‑6份，聚甲基丙烯酸甲酯和镁基金属微粉在135‑138℃温度下的羟基磷灰石粉表面形成含多种金属的“鸡尾酒”改性层结构。将镁基金属微粉在羟基磷灰石粉表面通过多次加热涂覆，形成“鸡尾酒”型复合结构，通过聚甲基丙烯酸甲酯的固定作用将镁基金属微粉固定到羟基磷灰石粉表面，提高羟基磷灰石粉与人体的结合强度、生物相容性和杀菌抗炎作用，能在口腔颌骨及牙槽骨缺损修复中起到良好的应用效果。
Description
技术领域
本发明涉及牙科植入材料加工与制备技术领域，尤其涉及一种“鸡尾酒”型成骨抗菌型骨粉及其制备方法。
背景技术
目前来源于生物体的成骨材料，包括自体骨材料和同种异体骨。自体骨有无排异、良好的骨诱导活性等众多优点，是植骨材料的金标准，但也有多个弊端—会给患者带来二次创伤、导致供骨区的功能缺失，且患者体质和年龄受限。同种异体骨来源相对充足，使用方便，但易引起免疫排斥反应而导致术后恢复失败。随着科技的发展及对BMP的深入研究，现已能在体外成功表达BMP。纯的BMP也有骨诱导的作用，但植入体内易被稀释及被蛋白酶分解，与骨形成周期不一致。目前市场上也有各种与BMP混合的复合物，BMP—羟基磷灰石，BMP—胶原等。但会出现体内不降解、诱导成骨不明显等问题，临床应用依然受限。
当材料植入机体后，其所含骨诱导因子BMP通过与间充质细胞中的受体与信号分子结合进行信号转导，在植入区局部发出基因调控信号，诱导间充质细胞分化成为软骨细胞及骨细胞。后经过软骨基质沉淀，血管长入，骨髓及骨髓腔分化形成等过程，最终诱导新骨形成。
申请号为201711405620.3的中国发明专利公开了一种PLA基牙科骨粉及其制备方法。该牙科骨粉的制备组分包含：左旋聚乳酸；矿化胶原，质量为左旋聚乳酸质量的50%～150%；多孔羟基磷灰石，质量为左旋聚乳酸质量的25%～30%；和卵磷脂，质量为左旋聚乳酸质量的5%～20%。制备方法包括：配制左旋聚乳酸溶液；共混；灌模；冻干；解析；粉碎；和筛分。其目的是实现良好的生物相容性和优异的亲水效果的PLA基牙科骨粉，改善骨修复效果，同时还具有良好的显影效果，其不足之处是生物稳定性和抑制细菌生长方面的特性不足，还有待改进。
发明内容
本发明的目的是提供一种“鸡尾酒”型成骨抗菌型骨粉及其制备方法，克服现有技术的不足，将镁基金属微粉在羟基磷灰石粉表面通过多次加热涂覆，形成“鸡尾酒”型复合结构，通过聚甲基丙烯酸甲酯的固定作用将镁基金属微粉固定到羟基磷灰石粉表面，提高羟基磷灰石粉与人体的结合强度、生物相容性和杀菌抗炎作用，能在口腔颌骨及牙槽骨缺损修复中起到良好的应用效果。
为实现上述目的，本发明的技术方案为：
技术方案之一：一种“鸡尾酒”型成骨抗菌型骨粉，其组分按重量份计包括：羟基磷灰石粉30-50份、聚甲基丙烯酸甲酯5-10份、镁基金属微粉3-6份，聚甲基丙烯酸甲酯和镁基金属微粉在135-138℃温度下的羟基磷灰石粉表面形成含多种金属的“鸡尾酒”改性层结构。
所述镁基金属微粉中的成分按质量百分比为：镍0.9%～2.1%，铬0.98%～1.20%，钼0.63%～0.70%，铜5.2%～8.5%，钒0.01%～0.03%，铌0.20%～0.30%，钙0.6%~0.8%，锌6%~7%，锶4%~5%，余量为Mg。
所述“鸡尾酒”改性层结构的表面粗糙度Ra为7~12μm，Rz为23~42μm，RSm为120~180μm，Rsk为0.46~0.75。
所述“鸡尾酒”改性层结构的孔隙率为35%~60%。
所述聚甲基丙烯酸甲酯的粒度为600目-900目，镁基金属微粉的粒度为600目-900目。
技术方案之二：一种“鸡尾酒”型成骨抗菌型骨粉的制备方法，具体操作步骤如下：
1）羟基磷灰石粉预处理，破碎、研磨，比表面积不低于350g/㎡；
2）将聚甲基丙烯酸甲酯与镁基金属微粉混合均匀；
3）将步骤1）和步骤2）所得物质混合，混合过程中逐渐升温到135-138℃，升温速率为20～35℃/min，在保温的状态下继续搅拌20~25分钟；
4）将步骤3）所得物质自然冷却至室温，粉碎至600目以下；
5）将步骤4）所得物质再与聚甲基丙烯酸甲酯和镁基金属微粉混合均匀，混合过程中逐渐升温到130-134℃，升温速率为36～40℃/min，在保温的状态下继续搅拌20~25分钟，所得物质自然冷却至室温，粉碎至600目以上，此步骤重复多次，直到使羟基磷灰石粉表面覆盖多层镁基金属微粉层，得“鸡尾酒”型成骨抗菌型骨粉。
步骤3）中在镁基金属微粉要分次填加到聚甲基丙烯酸甲酯粉末中。
步骤3)中搅拌在立式真空搅拌机中进行。
与现有技术相比，本发明技术方案的有益效果是：
1）镁（Mg）具有较高的负电极电位，与水发生化学反应而降解，被人体吸收及代谢，具有生物活性，可诱导细胞分化、生长和血管的长入，其作为植入器件植入生物体后，骨细胞向镁降解而减少的空间增殖、繁殖，随着镁逐步降解，形成新的具有原来特殊功能和形态的相应组织和器官，达到修复创伤和重建功能的目的。2）镁降解而形成的碱性环境能达到抑制细菌生长的目的。3）铜（Cu）离子来杀菌的历史悠久，有研究报道通过在纯钛中加入1%或5%的Cu元素，形成的Ti-Cu合金有明显的杀菌功能，并在动物体内植入实验中表现出了较强的抗炎症作用及一定的促进成骨的生物医学功能。3）将镁基金属微粉在羟基磷灰石粉表面通过多次加热涂覆，形成“鸡尾酒”型复合结构，通过聚甲基丙烯酸甲酯的固定作用将镁基金属微粉固定到羟基磷灰石粉表面，提高羟基磷灰石粉与人体的结合强度、生物相容性和杀菌抗炎作用，能在口腔颌骨及牙槽骨缺损修复中起到良好的应用效果。
附图说明
图1是本发明实施例1抗菌型骨粉形态示意图；
图2是本发明实施例1中纯羟基磷灰石粉（a），纯Mg粉（b），镁基金属微粉（c）与大肠杆菌共培养后的抗菌效果对比。
具体实施方式
下面将结合本发明实施方式中的附图，对本发明的实施方式中的技术方案进行清楚、完整的描述，显然，所描述的实施方式仅仅是作为例示，并非用于限制本发明。
以下实施例中，羟基磷灰石粉是采用水热合成法合成，以CaCO3和CaHPO4·2H2O为原料，在100 ℃的高压釜中经过10 h水热反应，制备出的晶粒完整的羟基磷灰石粉固体，其直径约80 nm。聚甲基丙烯酸甲酯的粒度为600目，镁基金属微粉的粒度为600目。镁基金属微粉中的成分按质量百分比为：镍1.6%～1.9%，铬1.1%～1.15%，钼0.65%～0.68%，铜6.5%～7.5%，钒0.02%～0.025%，铌0.25%～0.26%，钙0.7%~0.75%，锌6.2%~6.7%，锶4.2%~4.8%，余量为Mg。
实施例1
本发明一种“鸡尾酒”型成骨抗菌型骨粉的制备方法，取羟基磷灰石粉35份、聚甲基丙烯酸甲酯6份、镁基金属微粉5份，其具体操作步骤如下：
1）羟基磷灰石粉预处理，破碎、研磨，比表面积420g/㎡；
2）将聚甲基丙烯酸甲酯与镁基金属微粉混合均匀；
3）将步骤1）和步骤2）所得物质混合，混合过程中逐渐升温到135-138℃，升温速率为20～35℃/min，在保温的状态下继续搅拌20~25分钟；镁基金属微粉要分次填加到聚甲基丙烯酸甲酯粉末中。搅拌在立式真空搅拌机中进行，物料体积占搅拌机内容积的1/3~2/3，真空搅拌机内真空度为3 kPa~25kPa5；
4）将步骤3）所得物质自然冷却至室温，粉碎至600目；
5）将步骤4）所得物质再与聚甲基丙烯酸甲酯和镁基金属微粉混合均匀，混合过程中逐渐升温到132℃，升温速率为38℃/min，在保温的状态下继续搅拌25分钟，所得物质自然冷却至室温，粉碎至600目，此步骤重复3次，直到使羟基磷灰石粉表面覆盖4层镁基金属微粉层，得“鸡尾酒”型成骨抗菌型骨粉。“鸡尾酒”改性层结构的表面粗糙度Ra为10~12μm，Rz为30~42μm，RSm为150~160μm，Rsk为0.60~0.65，孔隙率为45%~50%。
见图1，本发明实施例1抗菌型骨粉形态示意图，聚甲基丙烯酸甲酯和镁基金属微粉在135-138℃温度下的羟基磷灰石粉表面形成含多种金属的“鸡尾酒”改性层结构，使用时，将本发明骨粉填充在口腔颌骨及牙槽骨缺损处的模型中，改性层与新成骨组织作用，形成新的骨质结构，达到修复创伤和重建功能的目的。
如图2所示，通过对纯羟基磷灰石粉（a），纯Mg粉（b），镁基金属微粉（c）与大肠杆菌共培养后的抗菌效果对比，本发明具有明显的抑菌作用。
实施例2
本发明一种“鸡尾酒”型成骨抗菌型骨粉的制备方法，取羟基磷灰石粉40份、聚甲基丙烯酸甲酯6份、镁基金属微粉4份，其具体操作步骤与实施例1相同。
实施例3
本发明一种“鸡尾酒”型成骨抗菌型骨粉的制备方法，取羟基磷灰石粉42份、聚甲基丙烯酸甲酯6份、镁基金属微粉3.5份，其具体操作步骤与实施例1相同。
实施例4
本发明一种“鸡尾酒”型成骨抗菌型骨粉的制备方法，取羟基磷灰石粉45份、聚甲基丙烯酸甲酯7份、镁基金属微粉5份，其具体操作步骤与实施例1相同。
实施例5
本发明一种“鸡尾酒”型成骨抗菌型骨粉的制备方法，取羟基磷灰石粉48份、聚甲基丙烯酸甲酯7份、镁基金属微粉4份，其具体操作步骤与实施例1相同。
上述实施例1－5所制得的成骨抗菌型骨粉，其与人体口腔颌骨及牙槽骨的结合强度、生物相容性和杀菌抗炎作用，在口腔颌骨及牙槽骨缺损修复中均取得良好的应用效果，优于常规的BMP混合的复合物，BMP—羟基磷灰石，BMP—胶原等复合骨粉。
当然，本发明还可以有其它多种实施例，在不背离本发明精神及其实质的情况下，熟悉本领域的技术人员可根据本发明作出各种相应的改变与变形，但这些相应的改变与变形都应属于本发明权利要求的保护范围。
Claims (8)
1.一种“鸡尾酒”型成骨抗菌型骨粉，其组分按重量份计包括：羟基磷灰石粉30-50份、聚甲基丙烯酸甲酯5-10份、镁基金属微粉3-6份，聚甲基丙烯酸甲酯和镁基金属微粉在135-138℃温度下的羟基磷灰石粉表面形成含多种金属的“鸡尾酒”改性层结构。
2.根据权利要求1所述的一种“鸡尾酒”型成骨抗菌型骨粉，其特征在于，所述镁基金属微粉中的成分按质量百分比为：镍0.9%～2.1%，铬0.98%～1.20%，钼0.63%～0.70%，铜5.2%～8.5%，钒0.01%～0.03%，铌0.20%～0.30%，钙0.6%~0.8%，锌6%~7%，锶4%~5%，余量为Mg。
3.根据权利要求1所述的一种“鸡尾酒”型成骨抗菌型骨粉，其特征在于，所述“鸡尾酒”改性层结构的表面粗糙度Ra为7~12μm，Rz为23~42μm，RSm为120~180μm，Rsk为0.46~0.75。
4.根据权利要求1所述的一种“鸡尾酒”型成骨抗菌型骨粉，其特征在于，所述“鸡尾酒”改性层结构的孔隙率为35%~60%。
5.根据权利要求1所述的一种“鸡尾酒”型成骨抗菌型骨粉，其特征在于，所述聚甲基丙烯酸甲酯的粒度为600目-900目，镁基金属微粉的粒度为600目-900目。
6.一种“鸡尾酒”型成骨抗菌型骨粉的制备方法，其特征在于，具体操作步骤如下：
1）羟基磷灰石粉预处理，破碎、研磨，比表面积不低于350g/㎡；
2）将聚甲基丙烯酸甲酯与镁基金属微粉混合均匀；
3）将步骤1）和步骤2）所得物质混合，混合过程中逐渐升温到135-138℃，升温速率为20～35℃/min，在保温的状态下继续搅拌20~25分钟；
4）将步骤3）所得物质自然冷却至室温，粉碎至600目以下；
5）将步骤4）所得物质再与聚甲基丙烯酸甲酯和镁基金属微粉混合均匀，混合过程中逐渐升温到130-134℃，升温速率为36～40℃/min，在保温的状态下继续搅拌20~25分钟，所得物质自然冷却至室温，粉碎至600目以上，此步骤重复多次，直到使羟基磷灰石粉表面覆盖多层镁基金属微粉层，得“鸡尾酒”型成骨抗菌型骨粉。
7.根据权利要求6所述的一种“鸡尾酒”型成骨抗菌型骨粉的制备方法，其特征在于，步骤3）中在镁基金属微粉要分次填加到聚甲基丙烯酸甲酯粉末中。
8.根据权利要求6所述的一种“鸡尾酒”型成骨抗菌型骨粉的制备方法，其特征在于，步骤3)中搅拌在立式真空搅拌机中进行。
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