该研究的目的是分析三种最近引入的预混生物陶瓷根管封闭剂的化学物理特性和生物活性(磷灰石形成能力),这些预混生物陶瓷根管封闭剂含有不同量的不同硅酸钙(CaSi):含硅酸二钙和三钙(1-10%和20-30%)的密封剂,含二氧化锆和铝酸三钙(CERASEAL);含硅酸三钙(5-15%)二甲基亚砜和碳酸锂(AHPLUSBIOCERAMIC)以及含硅酸二钙和硅酸三钙(10%和25%)的密封剂,含铝酸钙,铝酸三钙和钽酸盐(NEOSEALERFLO)。使用环氧树脂基密封剂(AHPLUS)作为对照。初始和最终设置时间,射线不透性,流动性,薄膜厚度,开孔体积,吸水,溶解度,钙释放和碱化活性进行了测试。通过ESEM-EDX评估了在汉克斯平衡盐溶液(HBSS)中老化28天后磷酸钙和/或磷灰石的成核,振动红外和显微拉曼光谱。分析显示,对于NeoSealerFlo和AHPlus,最终凝固时间最长(1344±60和1300±60分钟,分别),AH+生物陶瓷和Ceraseal的时间较短(660±60和720±60分钟,分别)。辐射不透明性,流动性和薄膜厚度符合ISO6876/12的所有测试材料。对于NeoSealerFlo,观察到明显更高的开孔体积,与AHPlus相比,AHPlus生物陶瓷和Ceraseal(p<0.05),在NeoSealerFlo和AHPlus生物陶瓷中观察到显着更高的值(p<0.05)。Ceraseal和AHPlus显示出最低的溶解度。所有含CaSi的密封剂释放钙并碱化浸泡水。在HBSS中浸泡28天后,ESEM-EDX分析显示形成了覆盖所有生物陶瓷密封剂表面的矿物层,放射性不透明剂的检测较低(用于Ceraseal和AHPlus生物陶瓷的锆,用于NeoSealerFlo的钽)和钙的增加,磷和碳。在NeoSealerFlo和AHPlus生物陶瓷上,磷酸钙(CaP)层更为明显。红外光谱和显微拉曼显示了碳酸钙在所有凝固材料的表面上的形成。仅在AHPlus生物陶瓷和NeoSealerFlo上检测到CaP相的薄层。尽管在所有测试的含CaSi的密封剂中,Ceraseal的钙释放最高,但未显示CaP沉积物。总之,含CaSi的密封剂满足所需的化学和物理标准并释放生物相关离子。观察到与高碳酸化过程有关的轻度/有限的磷灰石成核。
The aim of the study was to analyze the chemical−physical properties and bioactivity (apatite-forming ability) of three recently introduced premixed bioceramic root canal sealers containing varied amounts of different calcium silicates (CaSi): a dicalcium and tricalcium silicate (1−10% and 20−30%)-containing sealer with zirconium dioxide and tricalcium aluminate (CERASEAL); a tricalcium silicate (5−15%)-containing sealer with zirconium dioxide, dimethyl sulfoxide and lithium carbonate (AH PLUS BIOCERAMIC) and a dicalcium and tricalcium silicate (10% and 25%)-containing sealer with calcium aluminate, tricalcium aluminate and tantalite (NEOSEALER FLO). An epoxy resin-based sealer (AH PLUS) was used as control. The initial and final setting times, radiopacity, flowability, film thickness, open pore volume, water absorption, solubility, calcium release and alkalizing activity were tested. The nucleation of calcium phosphates and/or apatite after 28 days aging in Hanks balanced salt solution (HBSS) was evaluated by ESEM-EDX, vibrational IR and micro-Raman spectroscopy. The analyses showed for NeoSealer Flo and AH Plus the longest final setting times (1344 ± 60 and 1300 ± 60 min, respectively), while shorter times for AH Plus Bioceramic and Ceraseal (660 ± 60 and 720 ± 60 min, respectively). Radiopacity, flowability and film thickness complied with ISO 6876/12 for all tested materials. A significantly higher open pore volume was observed for NeoSealer Flo, AH Plus Bioceramic and Ceraseal when compared to AH Plus (p < 0.05), significantly higher values were observed for NeoSealer Flo and AH Plus Bioceramic (p < 0.05). Ceraseal and AH Plus revealed the lowest solubility. All CaSi-containing sealers released calcium and alkalized the soaking water. After 28 days immersion in HBSS, ESEM-EDX analyses revealed the formation of a mineral layer that covered the surface of all bioceramic sealers, with a lower detection of radiopacifiers (Zirconium for Ceraseal and AH Plus Bioceramic, Tantalum for NeoSealer Flo) and an increase in calcium, phosphorous and carbon. The calcium phosphate (CaP) layer was more evident on NeoSealer Flo and AH Plus Bioceramic. IR and micro-Raman revealed the formation of calcium carbonate on the surface of all set materials. A thin layer of a CaP phase was detected only on AH Plus Bioceramic and NeoSealer Flo. Ceraseal did not show CaP deposit despite its highest calcium release among all the tested CaSi-containing sealers. In conclusion, CaSi-containing sealers met the required chemical and physical standards and released biologically relevant ions. Slight/limited apatite nucleation was observed in relation to the high carbonation processes.