CN114681666A - 具备光热抗肿瘤和抗菌作用的骨修复材料及其制备方法 - Google Patents

具备光热抗肿瘤和抗菌作用的骨修复材料及其制备方法 Download PDF

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CN114681666A
CN114681666A CN202210142099.3A CN202210142099A CN114681666A CN 114681666 A CN114681666 A CN 114681666A CN 202210142099 A CN202210142099 A CN 202210142099A CN 114681666 A CN114681666 A CN 114681666A
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陈世杰
王栋
曾晋
彭毅
黄力平
仝昭宸
王卫国
李劲松
苗惊雷
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Third Xiangya Hospital of Central South University
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Abstract

本发明涉及骨修复材料，具体是具备光热抗肿瘤和抗菌作用的骨修复材料及其制备方法，其中骨修复材料包括聚多酚，还包括MBG粉粒、铜颗粒和石墨烯纳米颗粒，该石墨烯纳米颗粒吸附在铜颗粒表面形成复合颗粒，该复合颗粒负载于MBG粉粒上形成三元颗粒，所述聚多巴胺包覆在该三元颗粒外，得到包覆有聚多酚层的骨修复颗粒材料；该骨修复颗粒材料使铜颗粒具有光热转化功能，达到光热抗肿瘤的目的，且铜颗粒具有抗菌、促血管生成的作用；同时，本发明采用石墨烯纳米颗粒对铜颗粒进行改性以提高生物活性，高活性的铜颗粒与MBG粉粒复合可激活内皮细胞的HIF‑1α和TNF‑α通路，从而促进骨再生，实现骨修复。

Description

具备光热抗肿瘤和抗菌作用的骨修复材料及其制备方法
技术领域
本发明涉及骨修复材料，具体说是一种具备光热抗肿瘤和抗菌作用的骨修复材料及其制备方法。
背景技术
骨肿瘤是一种常见骨科疾病，临床上常采用外科手术切除和化疗的方法治疗。骨肿瘤切除后易造成大段骨缺损并残留部分肿瘤细胞。大段骨缺损难以自愈合，致残致畸率高；残留的肿瘤细胞易引起肿瘤再次复发。如何有效修复由骨肿瘤切除手术导致的骨缺损并杀死残留的肿瘤细胞是临床上骨肿瘤切除术后所面临的棘手问题。随着多功能生物材料的发展，光热治疗被广泛应用于肿瘤治疗及研究。在骨肿瘤领域研究中，将具备光热效应的组分与植入材料结合，使植入材料在近红外光照射下将光能转化为热能杀死肿瘤细胞。但现有的技术中，选用何种组分的光热材料及其如何制备、植入等还存在诸多的问题。
发明内容
针对上述技术问题，本发明提供一种可杀死剩余肿瘤细胞的同时促进骨缺损修复的具备光热抗肿瘤和抗菌作用的骨修复材料。
本发明解决上述技术问题所采用的技术方案为：具备光热抗肿瘤和抗菌作用的骨修复材料，其包括聚多酚，还包括MBG粉粒、铜颗粒和石墨烯纳米颗粒，该石墨烯纳米颗粒吸附在铜颗粒表面形成复合颗粒，该复合颗粒负载于MBG粉粒上形成三元颗粒，所述聚多巴胺包覆在该三元颗粒外，得到包覆有聚多酚层的骨修复颗粒材料。
作为优选，所述聚多酚由功能性基团与多巴胺或其衍生物聚合形成。
作为优选，所述的功能性基团为氨基团或巯基团。
作为优选，所述MBG粉粒的粒径为50-100μm，所述铜颗粒的粒径为5-10μm，所述石墨烯纳米颗粒的粒径为1-10nm。
作为优选，所述铜颗粒选自氧化铜、硫酸铜或氧化亚铜中的至少一种。
作为优选，所述聚多酚、MBG粉粒、铜颗粒、石墨烯纳米颗粒的质量比为1:（5-10）:（0.5-1）:（0.02-0.05）。
本发明还提供一种具备光热抗肿瘤和抗菌作用的骨修复材料的制备方法，其包括以下步骤：
（1）向铜颗粒中加入石墨烯纳米颗粒进行球磨；
（2）将球磨后的粉粒加入PVP溶液中，待石墨烯纳米颗粒吸附在铜颗粒表面后，再加入MBG粉粒进行超声分散，并搅拌均匀后进行离心分离，得到混合液；
（3）待上述混合液沉淀完全后，去上清液，并洗涤沉淀，得到三元颗粒；
（4）将上述三元颗粒加入由聚多酚配置的溶液中，反应完全后分离，获得包覆有聚多酚层的骨修复颗粒材料。
作为优选，所述聚多酚配置的溶液是由聚多酚、乙醇和氨水混合而成。
作为优选，将所述骨修复颗粒材料与复合水凝胶制成骨修复材料。
作为优选，使用戊二醛作为交联剂，羧基化的钠纤化纤维素和聚乙烯醇作为凝胶单体，制备出交联多孔的所述复合水凝胶。
从以上技术方案可知，本发明的包覆有聚多酚层的骨修复颗粒材料使其中的铜颗粒具有光热转化功能，达到光热抗肿瘤的目的；且铜颗粒具有抗菌、促血管生成的作用。同时，本发明采用石墨烯纳米颗粒对铜颗粒进行改性以提高生物活性，高活性的铜颗粒与MBG（介孔生物活性玻璃）粉粒复合可激活内皮细胞的HIF-1α（缺氧诱导因子-1α）和TNF-α（肿瘤坏死因子-α）通路，从而促进骨再生，实现骨修复。
具体实施方式
下面结合实施例详细介绍本发明，在此本发明的示意性实施例及说明用来解释本发明，但并不作为对本发明的限定。
本发明提供了一种具备光热抗肿瘤和抗菌作用的骨修复材料，其包括聚多酚，还包括MBG粉粒、铜颗粒和石墨烯纳米颗粒，该石墨烯纳米颗粒吸附在铜颗粒表面形成复合颗粒，该复合颗粒负载于MBG粉粒上形成三元颗粒，所述聚多巴胺包覆在该三元颗粒外，得到包覆有聚多酚层的骨修复颗粒材料；作为优选，所述聚多酚由功能性基团与多巴胺或其衍生物聚合形成，其中功能性基团为氨基团或巯基团等。由于聚多巴胺的特性，其可在含石墨烯-铜复合颗粒和MBG粉粒表面固定并形成包覆层，从而使复合颗粒表面带有氨基、巯基等官能团，不仅不会改变铜颗粒的光热转化属性，而且有利于与水凝胶、聚合物等材料结合，适合做骨修复材料。
本发明采用的MBG为无机材料，其与聚多巴胺等复合后可进一步增强聚多巴胺的亲水性能，提高生物相容性，且MBG降解后产物无毒无害，可被人体代谢。MBG由于孔隙的存在，不仅有利于负载复合颗粒，而且与水凝胶等制作成复合材料时，水凝胶分子会进入并吸附在孔隙内，从而改善材料的机械性能。同时，MBG可提供良好的细胞迁移、粘附的环境，其比表面积大，可增加负载药物量。在实施过程中，所述MBG粉粒的粒径为50-100μm，所述铜颗粒的粒径为5-10μm，所述石墨烯纳米颗粒的粒径为1-10nm。可见，石墨烯纳米颗粒与铜颗粒的粒径相差上千倍，铜颗粒表面巨大的表面能可牢牢吸附石墨烯纳米颗粒，形成石墨烯-铜复合颗粒，以实现对铜颗粒进行改性，提高生物活性；同时，MBG粉粒与复合颗粒之间也存在粒径差，加之MBG粉粒具有孔隙，很容易负载复合颗粒。
在实施过程中，所述铜颗粒选自氧化铜、硫酸铜或氧化亚铜中的至少一种。铜是人体必须元素，参与人体多种代谢过程，也是参与许多基本生物过程的重要微量营养素，表现出优异的抗菌、促血管生成、光热和抗氧化作用。本发明对含铜颗粒进行改性，通过与石墨烯纳米颗粒复合并负载在MBG粉粒上后外包覆聚多酚，可实现光热抗肿瘤的作用。高活性的石墨烯-铜复合颗粒作为骨修复材料通过光热转化释放后，可激活HIF-1α通路，并通过模拟缺氧环境或调节细胞内一氧化氮和钙的水平，可促进血管生成。同时本发明的铜与MBG粉粒复合后作为骨修复材料可激活人脐静脉内皮细胞的HIF-1α和TNF-α通路，从而促进骨再生，达到修复骨的目的。
作为优选，所述聚多酚、MBG粉粒、铜颗粒、石墨烯纳米颗粒的质量比为1:（5-10）:（0.5-1）:（0.02-0.05），不仅可达到改性铜颗粒的目的，而且可确保有足够的复合颗粒吸附在MBG粉粒上，也有足够的聚多酚分子包覆在三元颗粒上。石墨烯是一种良好的光热剂，可与多种小分子、聚合物发生交联，功能化方法简单；且石墨烯在体内外均具有良好的生物相容性，可与细菌充分接触、包裹，不会对正常组织、细胞产生强烈毒性，光热效率与抗菌效率高。本发明通过石墨烯纳米颗粒对铜颗粒进行改性，并与其他骨植入材料体系复合，可得到具备光热抗肿瘤及促成骨的抗菌复合材料，其光热效率与抗菌效率大大提高。
本发明还提供一种具备光热抗肿瘤和抗菌作用的骨修复材料的制备方法，其包括以下步骤：
首先，向铜颗粒中加入石墨烯纳米颗粒进行球磨，通过高速球磨可提高铜颗粒的机械活性，使铜颗粒与石墨烯纳米颗粒初步复合；然后，将球磨后的粉粒加入PVP溶液中，由此利用两者巨大的粒径差，使石墨烯纳米颗粒吸附在铜颗粒表面；再加入MBG粉粒进行超声分散，并搅拌均匀后进行离心分离，得到混合液；待上述混合液沉淀完全后，去上清液，并洗涤沉淀，得到三元颗粒；在PVP的保护下，利用MBG粉粒的孔隙和表面能使复合颗粒负载在MBG粉粒上，从而形成三元颗粒；接着将上述三元颗粒加入由聚多酚配置的溶液中，反应完全后分离，获得包覆有聚多酚层的骨修复颗粒材料。所述聚多酚配置的溶液是由聚多酚、乙醇和氨水混合而成，以保证聚多酚层包覆均匀，颗粒稳定。
本发明将上述骨修复颗粒材料与复合水凝胶制成骨修复材料，具体是使用戊二醛作为交联剂，羧基化的钠纤化纤维素和聚乙烯醇作为凝胶单体，制备出交联多孔的所述复合水凝胶。由于本发明制备的骨修复颗粒材料表面带有氨基、巯基等官能团，且可与高分子的复合水凝胶反应形成水凝胶网络结构并将骨修复颗粒材料包覆及固定在水凝胶网络中，增加了生物活性，可达到修改骨的目的。制成的骨修复材料在植入过程中由于降解或扩散等因素，可通过调控含铜颗粒的成分配比及制备工艺以调控光热效果及复合材料中铜离子释放速率等重要参数，以达到更好的抗肿瘤、抗菌及促成骨的作用。

Claims (10)

1.具备光热抗肿瘤和抗菌作用的骨修复材料，包括聚多酚，其特征在于：还包括MBG粉粒、铜颗粒和石墨烯纳米颗粒，该石墨烯纳米颗粒吸附在铜颗粒表面形成复合颗粒，该复合颗粒负载于MBG粉粒上形成三元颗粒，所述聚多巴胺包覆在该三元颗粒外，得到包覆有聚多酚层的骨修复颗粒材料。
2.根据权利要求1所述具备光热抗肿瘤和抗菌作用的骨修复材料，其特征在于：所述聚多酚由功能性基团与多巴胺或其衍生物聚合形成。
3.根据权利要求2所述具备光热抗肿瘤和抗菌作用的骨修复材料，其特征在于：所述的功能性基团为氨基团或巯基团。
4.根据权利要求1所述具备光热抗肿瘤和抗菌作用的骨修复材料，其特征在于：所述MBG粉粒的粒径为50-100μm，所述铜颗粒的粒径为5-10μm，所述石墨烯纳米颗粒的粒径为1-10nm。
5.根据权利要求1所述具备光热抗肿瘤和抗菌作用的骨修复材料，其特征在于：所述铜颗粒选自氧化铜、硫酸铜或氧化亚铜中的至少一种。
6.根据权利要求1所述具备光热抗肿瘤和抗菌作用的骨修复材料，其特征在于：所述聚多酚、MBG粉粒、铜颗粒、石墨烯纳米颗粒的质量比为1:（5-10）:（0.5-1）:（0.02-0.05）。
7.一种权利要求1至6中任意一项所述具备光热抗肿瘤和抗菌作用的骨修复材料的制备方法，其特征包括以下步骤：
（1）向铜颗粒中加入石墨烯纳米颗粒进行球磨；
（2）将球磨后的粉粒加入PVP溶液中，待石墨烯纳米颗粒吸附在铜颗粒表面后，再加入MBG粉粒进行超声分散，并搅拌均匀后进行离心分离，得到混合液；
（3）待上述混合液沉淀完全后，去上清液，并洗涤沉淀，得到三元颗粒；
（4）将上述三元颗粒加入由聚多酚配置的溶液中，反应完全后分离，获得包覆有聚多酚层的骨修复颗粒材料。
8.根据权利要求7所述具备光热抗肿瘤和抗菌作用的骨修复材料的制备方法，其特征在于：所述聚多酚配置的溶液是由聚多酚、乙醇和氨水混合而成。
9.根据权利要求7所述具备光热抗肿瘤和抗菌作用的骨修复材料的制备方法，其特征在于：将所述骨修复颗粒材料与复合水凝胶制成骨修复材料。
10.根据权利要求9所述具备光热抗肿瘤和抗菌作用的骨修复材料的制备方法，其特征在于：使用戊二醛作为交联剂，羧基化的钠纤化纤维素和聚乙烯醇作为凝胶单体，制备出交联多孔的所述复合水凝胶。
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