可注射非水相磷酸钙根管填充材料的研究
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摘要
根管治疗术是治疗牙髓病和根尖周病最有效的方法,而根充材料是决定其成败的关键因素。针对临床实际需求,本课题以与水互溶的非水相溶液为固化液,采用与粉末预先混合的方法制备出能在注射器中长期稳定保存而在体内快速固化的可注射非水相磷酸钙根充糊剂(Injectable nonaqueous calcium phosphate cement root canal filling paste, INCPCP)。
首先,制备了不同钙磷比的INCPCP,研究了钙磷比对体系理化性能的影响。随钙磷比升高,体系固化时间缩短,降解变慢。发现钙磷比为1.67的非水相CPC糊剂更符合根充材料的要求。通过对不同非水相固化液和颗粒粒径的CPC体系进行流变表征和稳定性分析,发现甘油,PEG600和丙二醇等三种INCPCP中,丙二醇体系粘度最低,易于注射；降低粒径可有效提高体系的悬浮稳定性。
其次,探讨了添加剂对INCPCP的改性作用。发现CTSAC提高了体系的显影性；1.5wt%磷酸氢二钠使体系固化时间从14小时缩短至4.5小时；1wt%ERHG使体系稳定性提高3倍。各添加剂的加入均不影响体系的固化。
与氢氧化钙糊剂相比,INCPCP在离体牙中能和牙本质紧密结合,根管封闭性好。细胞毒性实验表明体系具有良好的生物相容性。
本课题制备出的非水相CPC根充糊剂易注射,抗压强度较高,且具有适宜的固化时间和良好的悬浮稳定性,是一种应用前景良好的根充材料。
Root canal therapy (RCT) is an effective and fundmental treatment for pulposis. Properties of root canal filler determine the effects of root canal therapy. To meet the requirements of RCT, nonaqueous but water-soluble organic liquid and CPC powders were mixed to form a kind of premixed injectable nonaqueous CPC paste which is stable in syringe and hardens in vivo.
First, the injectable nonaqueous CPC with different Ca/P ratio was premixed as root canal filler. The effect of Ca/P ratio on physical and chemical properties was discussed. The result showed the setting time and degradation of filler decreased with increasing of Ca/P ratio and the CPC paste with Ca/p=1.67 behaved best as a root canal filler. The effects of different aqueous setting liquid and particle size on the rheology and suspension stability of CPC paste were also measured. The result showed among glycerol, propylene glycol and PEG600, paste with propylene glycol had low viscosity, which was fitted for injection. Reduction of particle size could effectively improve suspension stability.
Second, different additives were introduced into paste to improve the properties. The radiopacity of CPC pastes was improved by addition of CTSAC. The addition of 1.5wt% disodium hydrogen phosphate decreased the setting time form 14 hours to 4.5 hours.1%wt fumed silica increased suspension stability by 3 times.
In isolated teeth experiment, CPC pastes showed better sealing and were compacter with detine well than Ca(OH)2 pastes as control. Cytotoxicity results showed that CPC pastes were noncytotoxic and possess good biocompatibility.
CPC paste developed in this research could meet the requirements of root canal filling with a proper setting time, easy injection, improved suspension stability and high compressive strength. It is a kind of root canal filler with good perspective.
首先,制备了不同钙磷比的INCPCP,研究了钙磷比对体系理化性能的影响。随钙磷比升高,体系固化时间缩短,降解变慢。发现钙磷比为1.67的非水相CPC糊剂更符合根充材料的要求。通过对不同非水相固化液和颗粒粒径的CPC体系进行流变表征和稳定性分析,发现甘油,PEG600和丙二醇等三种INCPCP中,丙二醇体系粘度最低,易于注射；降低粒径可有效提高体系的悬浮稳定性。
其次,探讨了添加剂对INCPCP的改性作用。发现CTSAC提高了体系的显影性；1.5wt%磷酸氢二钠使体系固化时间从14小时缩短至4.5小时；1wt%ERHG使体系稳定性提高3倍。各添加剂的加入均不影响体系的固化。
与氢氧化钙糊剂相比,INCPCP在离体牙中能和牙本质紧密结合,根管封闭性好。细胞毒性实验表明体系具有良好的生物相容性。
本课题制备出的非水相CPC根充糊剂易注射,抗压强度较高,且具有适宜的固化时间和良好的悬浮稳定性,是一种应用前景良好的根充材料。
Root canal therapy (RCT) is an effective and fundmental treatment for pulposis. Properties of root canal filler determine the effects of root canal therapy. To meet the requirements of RCT, nonaqueous but water-soluble organic liquid and CPC powders were mixed to form a kind of premixed injectable nonaqueous CPC paste which is stable in syringe and hardens in vivo.
First, the injectable nonaqueous CPC with different Ca/P ratio was premixed as root canal filler. The effect of Ca/P ratio on physical and chemical properties was discussed. The result showed the setting time and degradation of filler decreased with increasing of Ca/P ratio and the CPC paste with Ca/p=1.67 behaved best as a root canal filler. The effects of different aqueous setting liquid and particle size on the rheology and suspension stability of CPC paste were also measured. The result showed among glycerol, propylene glycol and PEG600, paste with propylene glycol had low viscosity, which was fitted for injection. Reduction of particle size could effectively improve suspension stability.
Second, different additives were introduced into paste to improve the properties. The radiopacity of CPC pastes was improved by addition of CTSAC. The addition of 1.5wt% disodium hydrogen phosphate decreased the setting time form 14 hours to 4.5 hours.1%wt fumed silica increased suspension stability by 3 times.
In isolated teeth experiment, CPC pastes showed better sealing and were compacter with detine well than Ca(OH)2 pastes as control. Cytotoxicity results showed that CPC pastes were noncytotoxic and possess good biocompatibility.
CPC paste developed in this research could meet the requirements of root canal filling with a proper setting time, easy injection, improved suspension stability and high compressive strength. It is a kind of root canal filler with good perspective.
引文
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