Physicochemical properties of silicate tricalcium-based cement for use as pulp capping or repair materialAbstract
This study evaluated some physicochemical properties of an experimental tricalcium silicate-based cement (ETSC) indicated for use as pulp capping or endodontic repair material; Biodentine (BD) and White MTA-Angelus (MTA) cements served as comparators. Setting time, radiopacity, sorption, and solubility were determined according to ISO 6876/2012 and compressive strength according to ISO 9917-1/2019. pH and calcium ion release capacity were also assessed. Data were analyzed using ANOVA and Tukey tests or Kruskal-Wallis and Dunn tests with α = 0.05. BD (15’) and ETSC (17.3’) exhibited the shortest initial setting times, with BD (29’) having the shortest final setting time; MTA showed longer times in both analyses (p < 0.05). ETSC and MTA showed the highest radiopacity (6.1 mm Al and 5.7 mm Al), while BD showed the lowest (3.0 mm Al) (p < 0.05). BD exhibited the highest compressive strength (88.8 MPa), significantly higher than the others (p < 0.05). BD presented the lowest values for sorption, 0.12% (24 h) and 0.48% (28 d), which differed significantly from MTA (p < 0.05). The lowest values for solubility were shown for ETSC, 0.26% (24 h), and BD, 0.52% (28 d), which differed significantly from MTA (p<0.05). ETSC showed the highest pH throughout all periods; significant differences were observed for MTA (3 h) and BD (24 h) (p<0.05). In the Ca2+ analysis, BD provided the highest values in all periods; differences were only significant compared to MTA (3h/24h) (p <0 .05). Considering the study conditions, it can be concluded that ETSC exhibited characteristics similar or better properties than the commercial cements tested, except for compressive strength.
Dental Materials; Dental Pulp Capping
Introduction
In response to numerous scientific studies, dentistry has increasingly recognized the need for preventive treatments of a conservative nature, considered minimally invasive.1,2 These treatments aim to preserve teeth in the oral cavity for as long as possible and develop strategies to preserve pulp tissue vitality. To achieve this, the materials used should be biocompatible, stimulate the formation of mineralized tissue, and have suitable physical-chemical properties for use on both dentin and pulp tissue.3
Some bioceramic materials have been suggested for dental use as direct or indirect pulp capping in restorative dentistry and as repair materials in endodontics, due to their bioactivity.1,3,4 The use of these materials in dentistry marks a new phase in the treatment of deep caries, proposing a material with better physical properties than calcium hydroxide cement, which has traditionally been used as an indirect pulp capping material.5 Although it is known to stimulate the formation of mineralized tissue,5 calcium hydroxide cement has some undesirable properties for this purpose, such as high solubility,6 low sealing ability1 and low compressive strength.7
For the success of reparative and protective treatments of the dentin-pulp complex, the recommended material must have, among other physical-chemical characteristics, adequate setting time for manipulation and insertion, radiopacity, color stability, dimensional stability, compressive strength sufficient to withstand external masticatory forces,7 low solubility, good flowability, alkalinity, and the ability to release calcium ions.8
The first bioceramic material used in dentistry was a mineral trioxide aggregate introduced in the 1990s under the name ProRoot MTA (Dentsply-Tulsa Dental, Tulsa, USA).3 It consisted mainly of Portland cement, and its main components were tricalcium and dicalcium silicates, tricalcium aluminate, and tetracalcium ferroaluminate; calcium dihydrate sulfate and bismuth oxide were added as a setting retarder and radiopacifier, respectively.9 However, despite its good results, it had some drawbacks such as tooth discoloration, long setting time, and unsatisfactory handling characteristics.10
Over time, changes in the composition of the material were suggested. Gray Portland cement was replaced with white in an unsuccessful attempt to address the discoloration issue.9,11 Calcium dihydrate sulfate was removed from the composition, reducing the setting time;9,11 these changes gave rise to white MTA-Angelus (MTA; Angelus Ind. Prod. Odont. S/A, Londrina, Brazil). Its main components remained the same, but with a drastic reduction in tetracalcium ferroaluminate.
Another bioceramic material, Biodentine (BD; Septodont, Saint-Maur-des-Fossés, France), was introduced as a fast-setting bioactive cement, capable of replacing dentin.9,11 It contains tricalcium silicate instead of Portland cement, and zirconium oxide as radiopacifier. Changes in the composition have made it more applicable, with better mechanical properties,12 less induction of tooth discoloration,13 and a shorter setting time.14,15 However, this cement still has some disadvantages, such as reduced radiopacity,12,16 impossibility of portioning,17 and the need for a mechanical mixer since it is presented in pre-dosed capsules; cost can also be cited as a limitation.1
Despite these characteristics, Biodentine is difficult to access, opening an opportunity of developing a material that could combine good properties lower costs and an simpler application. In this sense, an experimental cement based on tricalcium silicate (ETSC) was developed. It is in powder/liquid form and contains in its powder tricalcium silicate (main component), zirconia oxide (radiopacifier), calcium oxide (expansion moderator/setting accelerator) and calcium phosphate (source of calcium and phosphorus). The liquid contains water, a high molecular weight hydrophilic polymer and a setting accelerator.
The progress that bioceramic materials have made to exhibit ideal characteristics for use in both endodontic and restorative dentistry is undeniable. Nevertheless, considering the limitations that still exist, the development of new bioactive materials that may overcome these limitations is important. Based on the above, the aim of this study was to evaluate the physical-chemical properties of setting time, radiopacity, compressive strength, sorption and solubility, pH, and calcium ion release capacity of an experimental tricalcium silicate-based cement, suggested for use as a direct pulp capping material and endodontic repair cement, comparing it to Biodentine and white MTA-Angelus cements. The null hypothesis of the study was that there are no statistically significant differences between the experimental cement and the evaluated commercial materials.
Methods
For the conduction of the tests, the commercial cements Biodentine and MTA-Angelus were provided and manipulated according to the manufacturer’s recommendations. The ETSC, which is in a powder-liquid form, was mixed manually with a #24 spatula on a polished glass slab at a ratio of 1:0.33 (g/g) for 1 minute. The basic compositions of the materials are described in Table 1.
Setting time
After manipulation, the cements were placed in metal rings with an inner diameter of 10 mm and a height of 2.0 mm (n = 3). The specimens were placed in an incubator at 37°C and 95% ± 5% relative humidity. A Gilmore-type needle with adjustable tip weight and diameter (Odeme Dental Research, Luzerna, Brazil) was used; a weight of 113.4 g with a 2 mm diameter tip was used to determine the initial setting time, and a weight of 453.6 g with a 1 mm diameter tip was used for the final setting time. Measurements were taken 180 seconds after the start of mixing until no indentations were visible on the specimen’s surface (ISO 6876/2012).
Radiopacity
Metal rings with internal diameter of 10.0 mm and height of 1.0 mm (n = 3) were filled with the manipulated materials and stored in an incubator at 37°C and 95 ± 5% relative humidity. After a time equal to three times the setting time, the rings were placed, along with an aluminum penetrometer (Odeme Dental Research), on an occlusal radiographic film (Kodak Comp, Rochester, USA). Radiographs were taken using an X-ray machine (Gnatus XR 6010; Gnatus, Ribeirão Preto, Brazil) with 60 kV, 10 mA, an exposure time of 0.3 seconds, and a focal distance of 30 cm (ISO 6876/2012). After developing the image, it was digitized, and radiopacity was measured using Image J software (NIH, Bethesda, USA). Radiopacity values were determined in millimeters of aluminum (mm Al) based on the radiographic density, converted using the formula proposed by Duarte et al.17.
Compressive strength
For compressive strength determination, specimens with a height of 3.58 mm and internal diameter of 3.0 mm were prepared (n = 10) and stored in an incubator at 37°C and 95% ± 5% relative humidity for 7 days.18-20 After this period, the specimens were removed from the molds and subjected to the compressive strength test in a universal testing machine (Instron #3345; Instron Inc., Canton, USA) at a speed of 1 mm/min. The maximum load required to fracture each sample was obtained and recorded. Compressive strength was calculated in megapascals (MPa) according to the equation: C = P/πr2, where “P” is the recorded maximum load in Newtons (N), “r” is the radius of the sample in millimeters (mm) (ISO 9917-1/2019).
Sorption and solubility
Sorption and solubility were evaluated after both 24 hours and 30 days of immersion, using separate samples for each period (ISO 9917-1/2019). For this purpose, Teflon rings with a diameter of 7.75 mm and height of 1.5 mm were filled with the cements (n = 6) and stored in an incubator at 37°C and 95% ± 5% relative humidity for three times the setting time. After the curing period, the masses of the specimens were measured on an analytical balance (± 0.0001 g) (BEL Equip. Anal. Ltda., Piracicaba, Brazil), and the values were recorded (M1). Subsequently, the specimens were placed in a desiccator and stored for 24 hours, after which they were measured again (M2). After the initial measurements, the specimens were immersed in 30 mL of distilled water and suspended on nylon threads for the analysis period. After 24 hours of immersion, the test specimens were removed from the vials, gently dried with absorbent paper, and new measurements were taken (M3); they were then kept in a desiccator for another 24 hours and a final measurement was taken (M4). Sorption was determined by the change in wet mass (M1–M3), and solubility was determined by the change in dry mass (M2– M4).
pH and calcium ion release
For pH and calcium ion release analysis determination, polyethylene tubes (n = 10) with a diameter of 1.0 mm and height of 10 mm, sealed at one end, were filled with the freshly manipulated materials.20 The tubes were immediately immersed in glass bottles previously treated with nitric acid and containing 10 mL of deionized water (Asfer Ind. Quim. São Caetano do Sul, Brazil); the initial pH was of 6.7. The bottles were placed in an incubator at 37°C and 95% ± 5% relative humidity and stored for 3, 24, 72, and 168 hours. At the end of each period, the polyethylene tubes with the materials were gently removed and immersed in new bottles. To eliminate bias, bottles with deionized water and empty polyethylene tubes were included in the sample as a control.
When determining the pH, the bottles containing the polyethylene tubes were mechanically agitated, and the pH of the liquid was analyzed using a digital pH meter (model #371; Micronal, São Paulo, Brazil) calibrated with control solutions. The analysis of calcium ions in the liquid was performed using a flame photometer (model #910-M, Tecnal Equip. Científicos, Piracicaba, Brazil); it employed a GLP gas flame maintained by compressed air. The apparatus was set to a wavelength of 554 nm and a slit width of 0.3 mm. Prior to the determinations, a standard curve was constructed from liquids with calcium concentrations close to those expected in the study.
Statistical analysis
The data collected throughout the study were first analyzed for normality using the Shapiro-Wilk test, indicating parametric and non-parametric results. Subsequently, depending on data distribution, ANOVA and Tukey tests (parametric – setting time, radiopacity and pH) with values reported as mean and standard deviation, or Kruskal-Wallis and Dunn tests (non-parametric – compressive strength, sorption, solubility and calcium ion release) with values reported as median and range (minimum and maximum). Regardless of the test applied, significance was set at α = 0.05.
Results
Table 2 presents the results of the evaluations of the physical-chemical properties, including setting time, radiopacity, and compressive strength. Biodentine and ETSC cements showed shorter initial setting times, around 15 minutes, with a significant difference from MTA-Angelus (p < 0.05). Regarding final setting time, Biodentine again had the shortest time, around 30 minutes, followed by ETSC and MTA-Angelus, with significant differences among the three materials (p < 0.05). The radiopacity value observed in ETSC (6.1 mm Al) was statistically similar (p > 0.05) to that obtained for MTA-Angelus (5.67 mm Al), and both were significantly higher than that of Biodentine (p < 0.05). However, all materials achieved a result equal to or greater than 3 mm of aluminum, as required by ISO 6876/2012. In terms of compressive strength evaluation, Biodentine provided better results compared to the other materials (88.8 MPa), with a significant difference from the other two materials (p < 0.05).
The data related to sorption and solubility analyses are listed in Table 3. All materials showed sorption at 24 hours and 28 days. MTA-Angelus had the highest sorption, increasing material mass by 5.61% (24 hours) and 6.72% (28 days), significantly higher than Biodentine at 24 hours and 28 days (p < 0.05). Solubility of MTA-Angelus was also significantly different at 24 hours and 28 days (p < 0.05), with negative values, indicating a gain in mass instead of mass loss as observed in the other materials, 2.11% (24 hours) and 3.64% (28 days). In the analysis of solubility at 24 hours, the materials met the parameters required by ISO 6876/2012, with values below 3%; however, at 28 days, MTA-Angelus showed a variation above this limit.
Table 4 presents the pH values for each material in different periods. The ETSC cement showed the highest pH values for the evaluated periods, 10.1, 9.96, 9.59, and 9.58. Statistically significant differences were found between EC and MTA-Angelus at the 3-hour mark and between EC and Biodentine at the 24-hour mark (p < 0.05). It is important to note that the pH value of the control remained at 6.78 throughout the study.
It was not possible to detect calcium in the control bottles. The values for the cements are available in Table 5. Biodentine cement provided the highest calcium release in the evaluated periods: 4.53 mg/dL, 5.26 mg/dL, 4.48 mg/dL, and 7.48 mg/dL. However, statistically significant differences were observed only between Biodentine and MTA-Angelus in the 3 and 24-hour periods (p < 0.05).
Discussion
The properties of dental materials are directly related to successful procedures. Actually, any currently available material can have all the desired characteristics for use as pulp capping or endodontic repair material. Therefore, the aim of this study was to formulate an experimental calcium trisilicate-based cement that exhibited physical-chemical properties closer to the ideal, but overcame the limitations of commercial cements previously mentioned. The observations in the present study demonstrated that the proposed experimental cement yielded results consistent with this indication. Its overall performance was similar to or better than that of the commercially available cements Biodentine and white MTA-Angelus, except for compressive strength. Thus, the initially suggested null hypothesis was rejected.
Regarding the methods used, the assessments of setting time and radiopacity followed the steps proposed by ISO 6876/2012. For the analysis of sorption and solubility, the same standard was followed, but notable adaptations were made, particularly in the dimensions of the specimens (7.75 mm in diameter and 1.5 mm in height), as suggested by Carvalho-Junior et al.18 and used in previous studies.19,22,23For the compressive strength test, ISO 9917-1/2019 was used, with adaptations in the dimensions of the specimens, as suggested by Carvalho-Junior et al.18 and later used by Bernardi et al.19 Another variation was the evaluation period, choosing an interval of 7 days, as recommended by Choi et al.24
The pH and calcium analyses were conducted according to the standard procedure commonly used in similar studies,25-28 but in this study a flame photometer was used instead of atomic absorption spectrophotometry, a method traditionally used for ion determination in fluids.29
A critical look at the setting time results reveals that the values of ETSC and Biodentine were similar and both were lower than those of MTA-Angelus. The times found for the commercial materials are consistent with those available in the literature.17,18 Setting time plays a crucial role in the use of the material, as it must gain strength as an intermediate material to allow for the placement of a temporary or definitive restoration.11 Given these findings, it is believed that the use of setting accelerators in the powder or liquid may have been responsible for the reduction in time to initial setting of the material; the use of pure tricalcium silicate instead of Portland cement, which is one of its components, may have also favored the reduction of time between handling and setting.14,17
Concerning the radiopacity results, the values obtained for ETSC and MTA-Angelus were important, as they showed highly satisfactory levels, close to 6 mm Al. This characteristic is especially important for the effective radiographic identification of the various dentin mineralization levels, intermediate material, and restorative material is required.16 However, the use of materials with greater or lesser radiopacifying capacity, as long as the standards are respected, is a clinical decision. The findings are consistent with the literature regarding the radiopacity levels of the tested commercial cements, once again highlighting the lower radiopacity exhibited by Biodentine.12,16,30
Better performance of compressive strength was observed for Biodentine, with significantly higher values compared to the other evaluated materials, which is consistent with the literature.12,31 Statistically similar values were found for the other two materials, and the results reported for MTA-Angelus were also in line with the literature.12,31 It is worth noting that the MPa values for all three tested materials were higher than the compressive strength values of calcium hydroxide cement,32 which has been widely used as an indirect pulp capping material.33 Another material that was widely used in the past as an intermediate and provisional restorative material was zinc oxide-eugenol cement, which, according to the study by Grech, Mallia, Camilleri12, showed compressive strength behavior comparable to silicate-based cements, being only inferior to Biodentine. This reinforces the suggestion of using the evaluated cements, including ETSC, as intermediate pulp capping materials. It is suggested that the high compressive strength values of Biodentine may be due to its resinous portion and the way it is mechanically manipulation, which ensures better mixing of the components.12,31
The analyses of sorption and solubility showed statistically similar behavior for Biodentine and ETSC, both experiencing low water sorption and solubility patterns at both 24 hours and 28 days, despite the large variation between minimum and maximum values. The findings for Biodentine are consistent with the available literature.12,31 However, MTA-Angelus exhibited high water sorption, possibly due to its porosity and hydrophilicity. Furthermore, the difficulty in “losing” this water was notable, as there was a percentage gain in mass rather than loss during immersion. This led to the suggestion of a microtomographic analysis of volume loss, but there is currently no standard or regulation for this type of observation.34
In the pH study, a pattern of alkalinizing potential was observed for all three materials tested, with values consistent with recent literature.25,27,28,30 ETSC stood out with the highest values throughout the study, surpassing the values of MTA-Angelus (at 3 hours) and Biodentine (at 24 hours). This factor may be important for the process of remineralization of the affected dentin tissue and for the elimination of microorganisms. However, further studies are required to confirm or refute these hypotheses. Parallel to this mechanism, the release of calcium ions is also important, as they can serve as centers for subsequent remineralization. In this regard, Biodentine and ETSC cements had the highest levels of calcium ion release, with Biodentine being superior to MTA-Angelus (at 3 and 24 hours) (p < 0.05). As for the levels found, the results of the present study are once again consistent with the available literature for commercial materials.25,27,28,30
In light of the findings reported here, it can be suggested that the experimental tricalcium silicate-based cement proposed in this study has physical-chemical properties that of offer good prospects for its use as a pulp capping or repair material. It also offers the possibility of portioning, ease manipulation and insertion, and a short setting time due to its powder/liquid presentation and the presence of hydrophilic polymers and a setting accelerator. Although it has comparable results to the evaluated commercial cements, Biodentine and white MTA-Angelus, further studies of a biological nature and clinical application tests are necessary to recommend it for use.
Conclusion
Under the conditions of this study, it can be concluded that the proposed experimental cement exhibited similar to or better results than the evaluated commercial materials, with the exception of compressive strength, where it showed lower values than Biodentine.
Acknowledgments
No potential conflict of interest relevant to this article was reported. This study was partially supported by Capes - Brazilian Federal Agency for Support and Evaluation of Graduate Education within the Ministry of Education of Brazil and Funcap - Ceará Foundation to Support Scientific and Technological Development.
References
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