目的:观察骨修复材料聚磷酸钙聚合度对其显微结构及体外降解性能的影响。 方法:实验于2006-02/05在四川大学组织工程支架材料研究室完成。通过控制煅烧时间制备得到具有不同聚合度的聚磷酸钙材料。使用液相^31P核磁共振法对聚磷酸钙聚合度进行测定。同时,采用X射线衍射仪及扫描电镜对试样进行表征。以生理盐水为递质,进行32d的体外降解实验,在不同时间使用钼蓝光度法对降解液中磷的质量浓度进行测定,降解过程中计算失重率:失重率(%)=[(W0-Wt)/W0]×100%。 结果:①聚磷酸钙聚合度随着煅烧时间(3,5,7,10h)的延长而增加,分别为9,13,17,19。②X射线衍射结果表明,聚合度对聚磷酸钙晶型无影响。③扫描电镜图片显示当聚合度大于9时,晶粒清晰可见。同时,晶界变薄,即非晶区变少。④32d体外降解实验结果表明,聚合度为13的聚磷酸钙材料的降解速率最快,失重率约是聚合度为9,19的3倍。 结论:不同聚合度的聚磷酸钙的显微结构不同并对其降解性能有一定影响,通过改变聚磷酸钙的聚合度从而调节其降解速率,配合其他影响因素对降解速率的调控可以达到满足临床骨修复要求。
AIM: To study the mechanism of controllable degradation of calcium polyphosphate (CPP) for bone repair, and observe the effect of polymerization degree on microstructure and in vitro degradation of CPP. METHODS: The experiment was performed at the Tissue Engineering Scaffold Materials Laboratory, Sichuan University from February to May 2006. CPP with different polymerization degree was prepared by controlling the calcining time. Average polymerization degree was analyzed by liquid state ^31p nuclear magnetic resonance (NMR). The samples were characterized by XRD and SEM. In order to evaluate the degradation of the glass ceramics prepared with different polymerization degree, degradation studies were carried out during 32 days in physiological saline solution. The rate of weight loss (%) = [(W0-W1)/W0]×100%. RESULTS: (1) The results of liquid state 31P NMR showed that the polymerization degree of CPP increased with the calcining time prolonging (3, 5, 7, 10 hours), which were 9, 13, 17 and 19 respectively. (2) X-ray diffraction (XRD) analysis demonstrated no significant difference of crystal system and space group of CPP with different polymerization degree. (3) The microstructure of CPP with different polymerization degree could be well distinguished at a magnification of x5000 by scanning electric microscope (SEM). (4) The results of 32-day in vitro degradation showed that the degradation velocity of CPP with polymerization degree=13 was three times more than other two samples. CONCLUSION: CPP of different polymerization degree has different microscope with certain effect on the degradation. The variation of polymerization degree by controlling the calcining time in the present study may be able to variation degradation velocity for clinical need.