林俊彬臺灣大學:臨床牙醫學研究所周芳如Chou, Fang-JuFang-JuChou2010-05-262018-07-092010-05-262018-07-092009U0001-0507200916143600http://ntur.lib.ntu.edu.tw//handle/246246/184169傳統根管封填材主要以馬來膠錐體搭配各類傳統封填劑，然而馬來膠錐體及各類傳統封填劑之間黏著力不足，和牙本質之黏著亦不理想，因此無法達到根管密封的目的。我研究團隊以樹酯為基底研發出聚胺酯根管封填系統，發現以PBA (polybutyleneadipate polyol)合成之聚胺酯根管封填材料在臨床操作而言有極佳的機械性質及熱性質，並且與牙本質有非常好的鍵結，可達良好密封性的目的，然而在材料接觸組織液的穩定性仍有疑慮，因此再研發以PC(polycarbonate polyol)合成之低水解聚胺酯根管封填材料。本研究目的主要在探討以PC合成之低水解封填系統材料的熱性質、機械性質及與根管牙本質間之鍵結強度，以及對聚胺酯根管封填系統材料及其他市售材料做細胞毒性及水解程度的評估。結果顯示以PC合成之聚胺酯錐體材料在熱性質方面熔點太接近體溫且稍微加熱後過於黏稠不利臨床操作；但以PC合成之胺酯壓克力樹酯封填劑在流動性是具臨床操作性的。在推離鍵結強度測試方面，以PC合成之胺酯壓克力樹酯與PBA合成之聚胺酯錐體材料的組合比其他市售材料有顯著較高的鍵結強度。在細胞毒性測試上，聚胺酯錐體在生物相容性優於馬來膠錐體，而PC合成之胺酯壓克力樹酯在完全聚合後生物相容性優於EndoREZTM，與AH plusTM相近，但PBA合成之胺酯壓克力樹酯在完全聚合後仍具細胞毒性，可能是起始劑所致。在水解程度的測試，PBA合成之聚胺酯錐體水解程度遠小於ResilonTM，而PBA及PC合成之胺酯壓克力樹酯封填劑皆有不錯的安定性。因此，依據各方面的測試，PC合成之胺酯壓克力樹酯與PBA合成之聚胺酯錐體在未來臨床根管治療的應用上深具潛力；而在PBA合成之胺酯壓克力樹酯及PC合成之聚胺酯錐體還有改善空間。Conventional root canal materials do not have enough dentinal adhesion and can not achieve the ideal sealing properties. Our research team has developed the polyurethane root canal obturation system containing ZnO/TPU cone and dual cured urethane acrylate(UA) sealer. Although these materials has good mechanical properties and bonding strength to dentin, the cytotoxicity and hydrolytic stability are questioned. The purposes of this study was to develop the low hydrolytic polyurethane root canal obturation system by replacing the PBA polyol with PC polyol and investigate the mechanical properties、bonding strength、cytotoxicity and hydrolysis of PBA and PC-based polyurethane root canal obturation system. The results showed that the PC-based ZnO/TPU cone can not be used in humen because the low melting point, but the PC-based urethane acrylate sealer fits the clinical use. In the push-out bonding test, the results revealed that PBA-based UA sealer/ PBA-based PU cone and PC-based UA sealer/PBA-based PU cone have the higher bonding strength than other commercial products. From cytotoxicity and hydrolysis evaluations, PBA-based ZnO/TPU cones have better biocompatibility than GP cones and much lower hydrolysis than ResilonTM. The PBA-based UA sealer has good stability to hydrolysis but has high cytotoxicity even in aged specimens. We estimate the reason is that the PBA-based UA sealer does not have good interaction with the AIBN and the residual AIBN causes the cytotoxicity. The PC-based UA sealer has good stability to hydrolysis and the cytotoxicity decreased at the fresh and aged specimens. We conclude that PBA-based ZnO/TPU cones and PC-based UA sealer have high potential for clinical use, and the thermal property of PC-based ZnO/TPU cone and the initiators of PBA-based UA sealer should be improved and changed.誌謝 ----------------------------------------------------------------------------------------------i文摘要 ----------------------------------------------------------------------------------------ii文摘要 ---------------------------------------------------------------------------------------iii寫表 ------------------------------------------------------------------------------------------ iv錄 ----------------------------------------------------------------------------------------------v次---------------------------------------------------------------------------------------------- ix次------------------------------------------------------------------------------------------------x一章 前言 ----------------------------------------------------------------------------------- 1二章 文獻回顧 ------------------------------------------------------------------------------5.1 理想的根管封填 ---------------------------------------------------------------------- 5.2 傳統根管封填材料的發展 ---------------------------------------------------------- 5.2.1 根管封填錐體材料 ---------------------------------------------------------------- 5.2.2 根管封填劑材料 ------------------------------------------------------------------- 7.3 近代根管封填系統的發展------------------------------------------------------------ 8.3.1 ResilonTM / EpiphanyTM 根管封填系統----------------------------------------- 8.3.2 EndoREZTM根管封填系統 ------------------------------------------------------ 11.4 聚胺酯材料作為高分子根管封填系統的潛力 --------------------------------- 12.4.1 熱塑型聚胺酯 -------------------------------------------------------------------- 12.4.2 本研究團隊初步試驗結果 ----------------------------------------------------- 13.5 根管填充材與根管牙本質間之鍵結強度測試 --------------------------------- 14.5.1 評估根管封填材料與根管壁間之黏著能力 -------------------------------- 15.5.2 推離鍵結測試法 ----------------------------------------------------------------- 15.6 生物相容性之測試--------------------------------------------------------------------17.6.1 MTT assay ---------------------------------------------------------------------------17 2.6.2 根管錐體材料毒性測試----------------------------------------------------------17 2.6.3 根管封填劑毒性測試-------------------------------------------------------------18 2.7 水解程度測試--------------------------------------------------------------------------19三章 動機與目的 ------------------------------------------------------------------------- 21四章 材料與方法 ------------------------------------------------------------------------- 23.1 PC合成之聚胺酯封填材實驗樣本之製備-----------------------------------------23.1.1 根管封填錐體材料 ---------------------------------------------------------------23.1.2 根管封填劑材料 ----------------------------------------------------------------- 23.2 熱分析試驗 --------------------------------------------------------------------------- 24.2.1 微差掃描熱量分析法 ----------------------------------------------------------- 24.3 機械性質拉力測試 ------------------------------------------------------------------ 25.3.1 拉力強度測試 - ------------------------------------------------------------------ 26.4 根管封填材與根管牙本質間之推離鍵結強度測試 --------------------------- 26.4.1 實驗樣本之製備 ----------------------------------------------------------------- 27.4.2 推離鍵結強度測試 -------------------------------------------------------------- 29.5 體外細胞毒性測試 ------------------------------------------------------------------ 30.5.1 3T3細胞培養 ---------------------------------------------------------------------- 30.5.2 錐體材料之準備工作 ----------------------------------------------------------- 31 4.5.2.1 錐體材料之樣本備製--------------------------------------------------------- 31 4.5.2.2 錐體材料之萃取液備製------------------------------------------------------ 31.5.3 封填劑材料之準備工作 -------------------------------------------------------- 31.5.3.1 封填劑材料之樣本備製------------------------------------------------------ 31 4.5.3.2 封填劑材料之萃取液備製--------------------------------------------------- 33.5.4 MTT assay--------------------------------------------------------------------------- 33.5.5 統計分析--------------------------------------------------------------------------- 34 4.6 材料水解測試------------------------------------------------------------------------- 34 4.6.1 酵素溶液之配製------------------------------------------------------------------ 34 4.6.2 實驗樣本之備製------------------------------------------------------------------ 35 4.6.3 實驗操作流程--------------------------------------------------------------------- 36 4.6.4 GPC測試---------------------------------------------------------------------------36五章 結果 ---------------------------------------------------------------------------------- 37.1 低水解聚胺酯封填錐體之測試結果 --------------------------------------------- 37.1.1 機械性質拉力強度測試之結果 ----------------------------------------------- 37.1.2 微差掃描熱量分析之結果 ----------------------------------------------------- 37 5.2 低水解胺酯壓克力樹酯封填劑之測試結果------------------------------------- 38 5.2.1 流動度測試------------------------------------------------------------------------- 38 5.2.2 硬化深度測試---------------------------------------------------------------------- 38.3 根管封填材與根管牙本質間之推離鍵結強度測試之結果------------------- 38.4 體外細胞毒性測試之結果---------------------------------------------------------- 39 5.4.1 錐體材料細胞毒性測試之結果------------------------------------------------- 39 5.4.2 封填劑材料細胞毒性測試之結果---------------------------------------------- 39.5 水解測試之結果---------------------------------------------------------------------- 40六章 討論 --------------------------------------------------------------------------------- 42.1 低水解聚胺酯封填錐體測試結果之探討-- ------------------------------------- 42.2 低水解胺酯壓克力樹酯封填劑測試結果之探討------------------------------- 42.3 根管封填材與根管牙本質間之推離鍵結強度測試之探討------------------- 43.4 體外細胞毒性測試之探討 --------------------------------------------------------- 43.4.1 錐體材料測試結果之探討------------------------------------------------------- 43.4.2 封填劑材料測試結果之探討 -------------------------------------------------- 45.5 水解測試結果之探討---------------------------------------------------------------- 46.5.1 水解實驗設計及評估方式之探討---------------------------------------------- 46.5.2 錐體材料水解程度之探討------------------------------------------------------- 47.5.3 封填劑材料水解程度之探討---------------------------------------------------- 49七章 結論 ---------------------------------------------------------------------------------- 51八章 未來研究方向 ---------------------------------------------------------------------- 52amp;#63851;考文獻 -------------------------------------------------------------------------------------- 53 次圖一 PC合成之熱塑型聚胺酯(TPU)和氧化鋅(ZnO)無機填充料複合材料之合成 -------------------------------------------------------------------------------------------62圖二 PC合成之胺酯壓克力樹酯 (urethane-acrylate, UA)封填劑之合成 -------------------------------------------------------------------------------------------63圖三 微差熱掃描分析儀 DSC 2010, TA Instruments -------------------------------64四 萬能拉力測試機 Universal Testing Instruments, RTM-IT ------------------64五 高速精密切割機 Isomet 2000 ----------------------------------------------------65六 馬來膠熱塑性封填系統 Warm gutta percha obturation system, E & Q Plus-----------------------------------------------------------------------------------65七 根管錐體材料熱充填儀器 Element® obturation unit ------------------------66八 高速鑽孔機 LT-848 ---------------------------------------------------------------66九 推離鍵結強度測試法流程圖------------------------------------------------------67十 錐體材料之萃取---------------------------------------------------------------------68十一 封填劑材料之萃取-----------------------------------------------------------------68十二 CE酵素及CE高濃度酵素溶液----------------------------------------------------69十三 材料在CE溶液內進行水解測試之狀況-----------------------------------------69十四 微差掃描熱量分析的結果---------------------------------------------------------70十五 PBS溶液水解測試結果-------------------------------------------------------------71十六 CE溶液水解測試結果--------------------------------------------------------------72十七 水解樣本觀察------------------------------------------------------------------------73 次一 推離鍵結強度測試之分組---------------------------------------------------------------74二 錐體材料體外細胞毒性之分組-------------------------------------------------------- 74 三 ISO 10993-5對萃取液萃取比例的規範-----------------------------------------------74四 封填劑材料體外細胞毒性之分組------------------------------------------------------75五 水解測試之分組---------------------------------------------------------------------------75六 PC合成之低水解錐體材料不同成分比例之機械性質-----------------------------75七 推離鍵結強度測試之結果---------------------------------------------------------------76八 錐體材料細胞毒性測試之結果---------------------------------------------------------76九 封填劑材料細胞毒性測試之結果------------------------------------------------------76十 水解樣本分子量之喪失比例------------------------------------------------------------77application/pdf1656376 bytesapplication/pdfen-US根管封填材料熱塑型聚胺酯胺酯壓克力樹酯推離鍵結強度測試細胞毒性水解Thermal polyurethanePush-out bonding testCytotoxicityHydrolysishttp://ntur.lib.ntu.edu.tw/bitstream/246246/184169/1/ntu-98-R95422003-1.pdf