目前, 傅里叶变换红外光谱(FTIR)技术具有待测样品数量少、 对特征基团灵敏度高、 样品制备和分析简单等优点; 电感耦合等离子体质谱(ICP-MS)的优势也较为显著: 微量元素的高灵敏度检出率, 低检测限和多元素的同时分析; 协同上述两种方法, 可快速对功能医用材料的化学元素和基团进行鉴定, 从而为仿生医用抗菌材料的研发提供新的设计思路和理论依据。 羟基磷灰石(HA)因其优异的骨传导和骨诱导特性被用于薄膜材料, 钛植入表面HA薄膜已进入临床应用阶段。 但是, HA的本真脆性和缺乏抗菌性, 常常导致植入失败。 因此, 开发一种耐磨性好且抑菌性优的促成骨功能涂层成为当前急需要解决的难题。 研究目的在于在钛表面制备耐磨性好且抑菌性优的促成骨功能涂层, 初步探讨了涂层的抗菌离子缓释规律和生物活性。 开拓性地在工业纯钛表面制备了明胶、 银和镁离子改性的羟基磷灰石(Mg-Ag-HA/明胶)抗菌涂层。 将银(Ag)引入羟基磷灰石涂层(HA)以改善其抗菌性能, 镁(Mg)作为第二元素以提高生物相容性, 明胶可以同时提高HA的生物相容性和力学性能。 ICP-MS测定涂层中镁和银元素的释放量和可持续性。 所得到的新型Mg-Ag-HA/明胶的SEM结果、 Ca/P比值、 化学特征峰和晶相通过FTIR, SEM, EDAX和XRD进行表征。 结果表明: 明胶的羧基与HA的钙离子之间已形成Ca—COO化学键, 明胶和Mg-Ag-HA构成了有机-无机复合涂层; Mg和Ag元素被成功地引入到了HA晶格中, 且分布均匀。 模拟体液浸泡后, Mg-Ag-HA/明胶涂层试样表面有新的缺钙型的HA生成, 且球形磷灰石中检测到新的Mg, Na和Cl元素; 结果表明, 新型复合涂层样品具有良好的生物活性。 SEM和LSCM实验结果观察发现, 小鼠颅骨成骨细胞在Mg-Ag-HA/明胶上粘附良好, 细胞伸展大量伪足, 未见细胞毒性。 明胶的加入大大降低了复合镀层中Mg2+和Ag+的释放速率, 提高了复合镀层的生理稳定性, 为镀层保持长期抗菌功能提供了保证。 Mg-Ag-HA/明胶作为钛基涂层材料具有良好的抗菌离子释放能力和优异的生物相容性, 为新型抗感染外科植入体的研发提供了新思路。

Fourier transform infrared spectroscopy (FTIR) has the advantages of a low test sample requirement, high sensitivity to characteristic groups and simple sample preparation and analysis. Inductively coupled plasma mass spectrometry (ICP-MS) is important because of its high detection rate sensitivity to trace elements, low detection limit and ability to analyse multiple elements simultaneously. Synergistically, the use of FTIR and ICP aids in the rapid identification of chemical elements and groups of functional medical materials, thereby providing new design ideas and theoretical basis for the development of bionic medical antibacterial materials. Hydroxyapatite (HA) is used in thin film materials because of its excellent bone conduction and osteoinductive properties. Titanium-implanted surface HA film is currently in the clinical application stage, but the brittleness and lack of antibacterial properties of HA often lead to implant failure. Thus, a bone-promoting functional coating with good wear resistance and excellent bacteriostasis must be developed to address these limitations. This paper presents a method for preparing a bone-promoting coating on the surface of titanium with good abrasion resistance and excellent bacteriostasis. The antibacterial ion sustained release law and biological activity of the coating were studied. For the first time, a gelatin, silver (Ag) and magnesium (Mg) ion-modified hydroxyapatite (Mg-Ag-HA/gelatin) antibacterial coating was prepared on the surface of industrial pure titanium. Ag was introduced into the HA coating to improve its antibacterial properties, while Mg was added to improve the biocompatibility of industrial pure titanium. Gelatin could simultaneously improve the biocompatibility and mechanics of HA. The release and sustainability of Mg and Ag in the coating were determined using ICP-MS. Morphology, Ca/P, chemical structure and crystal structure of deposited Mg-Ag-HA/gelatin were characterized using FTIR, scanning electron microscopy, electron diffraction spectroscopy and X-ray diffraction. Results showed that a Ca-COO chemical bond formed between the carboxyl group of gelatin and the calcium ion of HA. Gelatin and Mg-Ag-HA formed an organic-inorganic composite coating, and Mg and Ag were successfully introduced and evenly distributed into the HA lattice. After simulated body fluid immersion, a new calcium-deficient HA was formed on the surface of the Mg-Ag-HA/gelatin-coated samples, and new Mg, Na and Cl were detected in the spherical apatite. Results showed that the new composite coating has good biological activity. SEM and laser confocal experiments showed that mouse MC3T3-E1 cells adhered well on the film and had good morphology. The composite coating did not manifest cytotoxicity. The addition of gelatin greatly reduces the release rate of Mg2+ and Ag+ in the composite coating, improves the physiological stability of the composite coating and guarantees the long-term antibacterial function of the coating. As a titanium-based coating material, Mg-Ag-HA/gelatin has good antibacterial ion release ability and excellent biocompatibility, which provides a new idea for the development of new anti-infective surgical implants.