Story B J, Burgess A V, La D, Wagner W R
Sulzer Calcitek Inc., Carlsbad, California, USA.
J Biomed Mater Res. 1999;48(6):841-7. doi: 10.1002/(sici)1097-4636(1999)48:6<841::aid-jbm12>3.0.co;2-w.
A novel pressurized hydrothermal post-plasma-spray process has been developed to convert the crystalline non-HA and amorphous components of plasma-sprayed hydroxylapatite coatings back into crystalline HA. The process, known commercially as MP-1, was used to produce coatings comprising approximately 96% crystalline HA. The in vitro solubility of the coating in saturated citric acid solution has been measured to simulate the effect of implant detoxification procedures, which use citric acid as a cleaning medium. The MP-1 coating solubility in saturated citric acid solution (pH = 1) was compared to that of coatings with crystalline HA contents ranging from 37.5-82%. All coatings showed an initial sharp rise in coating dissolution, which correlated with crystalline HA content, followed by a steady state dissolution rate. After 60 s at 25 degrees C, the MP-1 coating showed a 65% decrease in solubility compared to a highly amorphous coating (AM-2). All coatings showed very similar steady state dissolution rates, except for AM-2, which was significantly higher. SEM analysis showed that the AM-2 coating surface was degraded substantially more than the other coatings, resulting in partial coating exfoliation. A mechanism of coating dissolution is proposed, in which the initial rapid leaching of soluble phases from the coating leaves behind a porous layer of highly crystalline HA at the coating surface. The stability of this porous crystalline layer leads to steady state, diffusion-limited dissolution of the remainder of the coating. The observed two-regime dissolution profile can be accurately represented by a 2-parameter model, which predicts the initial sharp rise in coating dissolution followed by a slower, steady state loss in coating mass. Model parameters were determined from experimental solubility data, and were shown to correlate with the percentage of crystalline HA in the coatings. The present data suggest that the treated coating is significantly more resistant to degradation from aggressive detoxification procedures such as citric acid burnishing.
已开发出一种新型的加压水热后等离子喷涂工艺,用于将等离子喷涂羟基磷灰石涂层中的结晶非羟基磷灰石和无定形成分转化回结晶羟基磷灰石。该工艺在商业上称为MP-1,用于生产包含约96%结晶羟基磷灰石的涂层。已测量了涂层在饱和柠檬酸溶液中的体外溶解度,以模拟使用柠檬酸作为清洁介质的植入物解毒程序的效果。将MP-1涂层在饱和柠檬酸溶液(pH = 1)中的溶解度与结晶羟基磷灰石含量在37.5 - 82%范围内的涂层的溶解度进行了比较。所有涂层在涂层溶解方面均显示出初始的急剧上升,这与结晶羟基磷灰石含量相关,随后是稳定的溶解速率。在25℃下60秒后,与高度无定形涂层(AM-2)相比,MP-1涂层的溶解度降低了65%。除AM-2涂层的溶解速率明显较高外,所有涂层的稳定溶解速率非常相似。扫描电子显微镜分析表明,AM-2涂层表面的降解程度明显高于其他涂层,导致部分涂层剥落。提出了一种涂层溶解机制,其中涂层中可溶性相的初始快速浸出在涂层表面留下了一层高度结晶的羟基磷灰石多孔层。该多孔结晶层的稳定性导致涂层其余部分的稳定、扩散受限溶解。观察到的双阶段溶解曲线可以由一个双参数模型准确表示,该模型预测涂层溶解的初始急剧上升,随后是涂层质量较慢的稳定损失。模型参数由实验溶解度数据确定,并显示与涂层中结晶羟基磷灰石的百分比相关。目前的数据表明,经过处理的涂层对柠檬酸抛光等侵蚀性解毒程序的降解具有显著更高的抗性。