Physicochemical properties of three bioceramic cements

Abstract:

This study aimed to compare the physicochemical properties of MTA Angelus (MTA-A), MTA Repair HP (MTA-HP), and Biodentine (BD). Setting times (n = 7) were determined in accordance with ASTM C266–15. Solubility (n = 11), pH (n = 10), and calcium ion release (n = 10) were evaluated up to 28 days in accordance with ANSI/ADA specification no. 57. Radiopacity was assessed by ANSI/ADA (n = 10) and the tissue simulator method (n = 10). In both methods, the specimens were radiographed using an aluminum stepwedge and the digital radiographs were analyzed in Adobe Photoshop, determining the mean grayscale pixel values of the materials, of the 3-mm aluminum stepwedge, and of the dentin, the latter of which was analyzed on the tissue simulator. The data obtained from each test were statistically analyzed and compared (p < 0.05). MTA-A presented longer final setting time compared with the other materials. There were no significant differences in the mass values of materials during the experiment. All materials presented an alkaline pH. BD promoted greater calcium ion release in most of the experimental periods. All materials presented appropriate radiopacity. BD showed lower radiopacity than MTA-A in the tissue simulator method. All groups presented higher radiopacity in the tissue simulator when compared with the ANSI/ADA method. MTA-A, MTA-HP, and BD showed appropriate physicochemical properties and radiopacity, and were considered suitable to be used in clinical practice.

Keywords:
Endodontics; Biocompatible Materials; Root Canal Filling Materials; Dental Materials

Introduction

Mineral trioxide aggregate (MTA) had been initially developed for sealing root perforations and as a root-end filling material.¹ Due to its physicochemical¹ and biological² properties, it has been also indicated for vital pulp therapy² as an apical plug³ and as a coronal barrier in the endodontic treatment of immature teeth.⁴ MTA formulation comprises a powder – containing tricalcium aluminate, tetracalcium aluminoferrite, calcium sulfate, gypsum, and bismuth oxide – and distilled water.⁵ White MTA Angelus (MTA-A) is slightly different from the original MTA, with a lower content of tetracalcium aluminoferrite and calcium sulfate.⁶ More recently, bismuth oxide has been replaced with calcium tungstate as radiopacifier to avoid tooth discoloration from the reaction of bismuth oxide with sodium hypochlorite and/or dentin collagen,⁷ but the physicochemical properties of the new formulation still have to be studied.

Besides the risk of tooth discoloration, difficulties with handling⁸ have encouraged the development of alternative materials. MTA Repair HP (MTA-HP) (Angelus, Londrina, Brazil) has been developed to provide higher plasticity. The main difference from the most recent formulation of MTA-A is the addition of an organic plasticizer to distilled water⁹. Recent studies have demonstrated that MTA-HP improves resistance to dislodgement and flowability,⁹ maintaining the widely acclaimed biological properties of MTA.⁶ However, other physicochemical properties of this material, including radiopacity, should be further investigated.

Biodentine™ (BD) (Septodont, Sair Maur de Fossés, France) is another alternative to MTA. It contains tricalcium silicate, dicalcium silicate, calcium carbonate, iron oxide, and zirconium oxide (powder), in addition to a liquid with calcium chloride (accelerator), water-soluble polymer, and a water-reducing agent.¹⁰ Greater microhardness and resistance to compressive loading are some of the advantages of BD in comparison with MTA.¹¹ Studies evaluating biological properties¹² and antimicrobial activity¹³ have also indicated favorable properties. On the other hand, there is no consensus on the radiopacity of BD when the ANSI/ADA method¹⁴,¹⁵ is used; therefore, additional methods that evaluate radiopacity under the influence of osseous, dental, and soft tissue superimposition should be considered.¹⁶

In the standard method, the absence of tooth, bone, and soft tissue could alter the perception of radiopacity in dental materials, thus requiring the addition of radiopacifier to their compositions, potentially influencing other properties.¹⁶,¹⁷ Previous studies have shown higher radiopacity of endodontic sealers using the tissue simulator block,¹⁷,¹⁸ but to date, this method has not been used to evaluate bioceramic materials.

The present study aimed to compare baseline and final setting times, pH, solubility, and calcium ion release of MTA-A, MTA-HP, and BD. Moreover, the radiopacity of these materials was evaluated both by the ANSI/ADA and the tissue simulator methods.

Methodology

This study was approved by the local research ethics committee (protocol nº 2.940.053). Setting time, solubility, pH, release of calcium ions and radiopacity of MTA-A (Angelus, Londrina, Brazil), MTA-HP (Angelus, Londrina, Brazil), and BD (Septodont, Sair Maur de Fossés, France) were evaluated. All materials were prepared according to the manufacturers’ instructions. The sample size was determined for each experiment by means of a calculation based on the results of previous studies.¹⁶,¹⁷,¹⁹ BioEstat 5.0 statistical package (Mamirauá Foundation, Belém, Brazil) was used.

Setting time

The baseline and final setting times were evaluated according to ASTM C266–15 and ISO 6876:2012.²⁰ Plaster molds (n = 7) with an internal diameter of 10 mm (± 0.1 mm) and a height of 2 mm (± 0.1 mm) were filled with the mixed material. The specimens were maintained for 5 min in an incubator at 37°C with a relative humidity of 99 ± 5% before the baseline setting time measurements. Baseline setting time was measured with a Gillmore needle (diameter of 2 mm (± 0.1 mm), height of 5 mm, and weight of 100 g (± 5 g)) carefully lowered onto the surface of the specimen without any further pressure. This procedure was repeated every 60 s until an impression was no longer visible on the material surface, and the baseline setting time was then recorded. The final setting time (time elapsed from the beginning of mixing to the time at which no indentation was detected on the surface of the specimens) was determined with a larger Gillmore needle (diameter of 1 mm (± 0.1 mm) and weight of 456.5 g (± 5 g)).

Solubility

The solubility test (n = 11) was adapted from the American National Standard Institute/American Dental Association (ANSI/ADA) specification no. 57/2000²¹ and ISO 6876:2012.²⁰ MTA-A, MTA-HP, and BD specimens were prepared using plastic molds with a height of 1.5 mm (± 0.1 mm) and an internal diameter of 7.75 mm (± 0.1 mm), as proposed by Carvalho-Júnior et al.²² The molds were placed on a glass plate and filled with the mixed material. Another plate was positioned over the specimens and then stored in an incubator at 37°C with a 95% relative humidity, using a setting time three times longer than at baseline, as recommended by the manufacturers (12 min for MTA-A and MTA-HP, and 15 min for BD). The specimens were unmolded and weighed on a precision scale with an accuracy of 0.001g (Sartorius 1801MPS, Göttingen, Germany) to determine their initial mass (P-0). After the baseline weight measurements, the specimens were immersed in 15-mL Falcon tubes (Labor Import, Osasco, São Paulo, Brazil), filled with 7.5 mL of deionized water, and maintained in the incubator (SXCR80, Sterilifer Ind. Com. Ltda., Diadema, Brazil) for 24 h. Subsequently, the specimens were removed from the incubator, slightly dried with absorbent papers, and placed in a drying chamber at 37 °C for 48 h. The specimens were then weighed in 72-hour shifts for 28 days. The specimens were maintained in the incubator throughout the weight measurements. Solubility was obtained by calculating the mass loss after the experimental periods in comparison with P-0.

pH and calcium ion release

For pH and calcium ion release analysis (n = 10), MTA-A, MTA-HP, and BD were inserted into 10 x 1.6-mm polyethylene tubes. After the baseline setting time (provided by the manufacturers), the specimens were inserted into 50-mL Falcon tubes (Cral Artigos para Laboratório Ltda, Cotia, São Paulo, Brazil.) containing 10 mL of deionized water (pH = 7.4). The specimens were stored at 37°C during the experimental period. The storage water was replaced at each endpoint (1, 3, 12, and 24 h and 7, 14, 21, and 28 days), and the collected water was analyzed for pH by using a pH meter (Digimed, Digicrom Analitica, Campo Grande, Brazil), previously calibrated with standard solutions with known pH (4 and 7). The calcium ion release assessment was performed in the same experimental periods used for pH analysis. The calcium levels of the collected specimen were analyzed by the colorimetric method using Arsenazo III.²³

Radiopacity

The radiopacity of MTA-A, MTA-HP, and BD was evaluated by two methods. In the ANSI/ADA method (n = 10), the materials were prepared and placed in acrylic plates containing 4 x 1.5-mm rings. The filled rings were stored at 37°C (± 1) in 95% (± 5) humidity for 7 days until the materials were completely set. Afterwards, the specimens were radiographed using a phosphor plate²⁴,²⁵ and an aluminum stepwedge.

Radiopacity was further evaluated using the tissue simulator developed by Gegler and Fontanella.¹⁶ Briefly, to build the simulator, the maxillary anterior region of a human skull was split by sagittal osteotomy into two segments fixed with wax (Wilson, São Paulo, Brazil) in a plastic container (length of 56 cm; width of 52.5 cm; depth of 53.5 cm). Distances of 1 cm were established between the external surfaces of the buccal and palatal segments and the container walls. This space was filled with self-curing acrylic (Artigos Odontológicos Clássico, São Paulo, Brazil) that could simulate the soft tissues. A distance of 0.5 cm was established between the internal surface of the buccal bone and the internal surface of the palatal bone. The space was filled with wax, which was used to fix a human canine root with the previously prepared root canal. The root was inserted up to the point at which the cementum-enamel junction coincided with the level of the alveolar crest. To evaluate radiopacity in this tissue simulator, the materials were manipulated and introduced into polyethylene tubes (length of 10 mm and diameter of 1.5 mm; Abbott Lab do Brasil, São Paulo, Brazil) with a syringe to avoid bubbles (n = 12 for each cement). The filled tubes were stored at 37°C (± 1) in 95% (± 5) humidity for 7 days until the materials were completely set. Thereafter, they were individually placed in the root canal of a canine tooth in the tissue simulator and radiographed using a phosphor plate and an aluminum stepwedge (Figure).

Figure
(A) Tissue simulator. Acrylic block simulating soft tissues and containing a fragment of osseous tissue (a) and a canine tooth (b) involved by utility wax to simulate periodontal ligament (c). (B) Polyethylene tubes into which the bioceramic cements were inserted. (C) Radiographic image of a polyethylene tube filled with Biodentine and inserted into a canine tooth in the tissue simulator, in addition to an aluminum stepwedge.

In both methods, the radiographs were obtained using a radiographic unit (Timex 70C, Gnatus, Ribeirão Preto, Brazil) operating at 70 kV and 10mA, with a 0.1-s exposure time and a 30-cm focal distance set. The images were generated using a scanner (Dürr Dental SE) and then exported and saved in JPG format. The digital images were analyzed using Adobe Photoshop® CS5 (Adobe Systems, San Jose, USA). For the images obtained with the ANSI/ADA method, a standard-size square (400 pixels) was drawn at the center of the standard disc (material), and another one was drawn in the third step, from left to right, of the aluminum stepwedge, equivalent to 3 mm of aluminum. In the simulator method, three standard-size squares (400 pixels) were drawn: one under the tube containing the material, another one under the dentin (both in the bone tissue overlap region), and the third one in the aluminum stepwedge at the same step described above. The mean and standard deviation of the grayscale pixel values of each selected area were measured and recorded using the histogram tool.

Data analysis

The statistical analysis was performed with GraphPad Prism 5.0 (GraphPad Software, San Diego, USA) (α = 0.05). Baseline and final setting times were compared amongst the experimental groups using one-way ANOVA and Tukey's post-hoc test. The solubility of each material was evaluated throughout the experiment using repeated-measures ANOVA and Tukey's post-hoc test. Calcium ion release and pH were compared amongst the groups and the experimental periods by two-way ANOVA and Tukey's post-hoc test.

In both methods tested herein, radiopacity was compared amongst the groups using one-way ANOVA and Tukey's post-hoc test. The minimum radiopacity recommended by ANSI/ADA for the aluminum stepwedge (equivalent to 3 mm of aluminum) was used as a control for both methods. Besides, in the tissue simulator, dentin radiopacity was also used as a control. To compare the methods, the data were evaluated by Student's unpaired t-test.

Results

Baseline and final setting times of all tested materials are shown in Table 1. MTA-A presented a longer final setting time compared with MTA-HP and BD (p = 0.0001). There was no significant difference when evaluating the variability of mass values in the solubility test (p < 0.05). All the tested materials presented an alkaline pH – close to 10 – during the experimental period. After 1 h, MTA-HP presented a more alkaline pH in comparison with MTA-A (p < 0.05). Both MTA-HP and MTA-A showed significantly greater calcium ion release after 21 days, while BD presented greater release of calcium ions from the third day (p < 0.05). BD promoted greater calcium ion release in most of the experimental periods, except after 1 h and 14 and 28 days (p < 0.05) (Table 1).

Table 1
Mean and standard deviation (± SD) of initial and final setting times (minutes), solubility expressed as mass loss (%) in relation to initial mass (g) and pH values measured in different experimental periods of MTA HP, BD and MTA-A.

Variable		MTA-HP	BD	MTA-A
Setting time
	Initial (min)	19.14 ± 1.46aA	21.71 ± 1.60aA	18.71 ± 8,60aA
	Final (min)	35.86 ± 2.19aB	33.29 ± 4.31aB	44.43 ± 2.82bB
Solubility
	m-0	0.16 ± 0.01aA	0.17 ± 0.02aA	0.18 ± 0.01aA
	m-1	0.17 ± 0.01aA	0.15 ± 0.05aA	0.20 ± 0.22aA
	m-2	0.17 ± 0.01aA	0.16 ± 0.01aA	0.20 ± 0.22aA
	m-3	0.16 ± 0.05aA	0.16 ± 0.01aA	0.20 ± 0.02aA
	m-4	0.17 ± 0.01aA	0.16 ± 0.01aA	0.20 ± 0.02aA
	m-5	0.17 ± 0.01aA	0.16 ± 0.01aA	0.20 ± 0.02aA
	m-6	0.17 ± 0.01aA	0.16 ± 0.01aA	0.19 ± 0.02aA
	m-7	0.17 ± 0.01aA	0.16 ± 0.01aA	0.19 ± 0.02aA
pH
	1h	10.11 ± 0.4aA	10.14 ± 0.14abA	9.82 ± 0.10bA
	3h	10.28 ± 0.13aA	10.50 ± 0.44aA	10.31 ± 0.09aA
	12h	10,16 ± 0,25 aA	10,26 ± 0,46aA	10,28 ± 0,21aA
	12h	10,16 ± 0,25ABCa	10,26 ± 0,46Aba	10,28 ± 0,21BCa
	24h	10.20 ± 0.34aA	10.19 ± 0.60aA	10.27 ± 0.27aA
	7 days	10.33 ± 0.50aA	10.52 ± 0.62aA	10.55 ± 0.20aA
	14 days	10.68 ± 0.41aA	10.87 ± 0.64aA	10.99 ± 0.1aA
	21 days	10.86 ± 0.58aA	10.83 ± 0.74aA	10.92 ± 0.28aA
	28 days	10.87 ± 0.54aA	10.79 ± 0.74aA	10.76±0.45aA
Calcium ions release
	1h	335.63 ± 102.56aA	383.70 ± 30.77aA	397.95 ±104.75abA
	3h	371.46 ± 24.70aA	384.34 ± 11.34bB	328.66 ± 42.13aA
	12h	349.96 ± 34.05aA	383.19 ± 7.16bB	337.15 ± 23.14aA
	24h	333.08 ± 48.43aA	422.70 ± 5.44bC	329.48 ± 51.54aA
	7 days	400.28 ± 26.40aA	433.84 ± 8.07bB	403.65 ± 20.73aA
	14 days	482.38±41.5aA	421.55 ± 7.15bB	414.22 ± 9.39abA
	21 days	573.56 ± 18.77aB	591.95 ± 2.07bD	576.73 ± 23.26aB
	28 days	570.87 ± 51.79aB	579.83 ±50.31aB	559.55 ± 60.30aB

• ^*
  Different lowercase letters in each row indicate significant difference amongst experimental groups (p < 0.05). Different capital letters in each column indicate significant differences among experimental periods (p < 0.05).

Table 2 summarizes the findings on radiopacity. All tested bioceramic cements showed higher radiopacity in the tissue simulator method as compared to the ANSI/ADA method (p < 0.05). In both methods, all materials presented higher radiopacity than 3 mm of aluminum stepwedge. In the tissue simulator, the three tested materials presented higher radiopacity than dentin. There were no significant differences amongst the materials when evaluating radiopacity through the ANSI/ADA method, while BD showed lower radiopacity than MTA-A when materials were evaluated in the tissue simulator (p < 0.05).

Table 2
Means and standard deviation of MTA-HP, BD, and MTA-A radiopacity (in grayscale pixel) (n = 10 per group).

Variable	ANSI/ADA		Tissue Simulator		Dentin
	Material	AL	Material	AL
MTA-HP	91.95 ± 17.81Aa	83.50 ± 10.01Ab	192,5 ± 1.75Bab	153,12 ± 0.88Bd	181,17 ± 1.05c
BD	94.38 ± 5.12Aa	85.50 ± 10.00Ab	191,1 ± 3.21Ba	149,35 ± 0.90Bd	180,10 ± 0.88c
MTA-A	98.35 ± 12.9Aa	88.10 ± 09.34Ab	194,3 ± 1.37Bb	157,13 ± 0.78Bd	182,68 ± 0.98c

• Values with different superscript uppercase letters represent statistically significant differences between the radiopacity evaluation methods. Values with the same superscript lowercase letters were not statistically different when comparing the groups (p < 0.05).

Discussion

In the present study, the physicochemical properties of MTA-A, MTA-HP, and BD were investigated. Baseline setting time was evaluated to observe the suitability of the tested materials in clinical procedures performed in a single appointment, since a faster setting time reduces dislodgement after material placement.²⁶ The original MTA set after 2 h and 45 min¹, which has traditionally been considered a drawback. In agreement with previous studies,⁹,²⁷ the three tested materials showed adequate baseline setting time – about 20 minutes –, which was similar among the materials. Modifications in the original formulation such as absence of calcium sulfate²⁸ and bismuth oxide⁹ have probably influenced this outcome.

With regards to the new formulation of MTA-A, although the values of baseline setting time were very similar to those found in other studies that have evaluated MTA-A with bismuth oxide,⁹,²⁷ the final setting time was longer in comparison with that of the other materials, probably due to differences in the formulations of the materials. MTA-HP differs from MTA-A mainly in the liquid component. The organic plasticizer of MTA-HP could have altered the water content after the mixing process, thus affecting setting time. In this regard, setting time is directly affected by moisture.²⁴ Moreover, higher surface area has been previously observed for MTA-HP in comparison with MTA-A, which correlates with smaller particle sizes and could accelerate the setting time.²⁹ In BD, the addition of calcium chloride in the liquid component has probably reduced the setting time.³⁰ Accordingly, it has been previously observed³⁰ that the use of calcium chloride is efficient in accelerating the setting of bioceramic materials.

Solubility and contamination before complete setting are concerns for materials with a longer final setting time.²⁶ On the other hand, the differences observed herein did not seem to affect MTA-A solubility. As a matter of fact, there were no significant differences in solubility amongst the materials throughout the experiment. The three silicate-based cements showed constant mass values and presented appropriate behavior - in accordance to ISO 6876²¹ - proving their suitability as root repair materials, when in contact with body fluids. Calcium tungstate is insoluble in water, contributing to MTA-A and MTA-HP insolubility.⁶

An ideal bioceramic material should have alkaline pH and calcium ion release as early as possible, and these environmental conditions should be maintained for long periods. In this regard, an alkaline pH should contribute to the maintenance of an environment that is inhospitable to microbial growth²⁴,²⁶ and, together with the presence of calcium ions, favor the mineralization process.¹²,¹³ In the current study, MTA-HP showed greater pH than MTA-A after 1 h, but all the bioceramic materials sustained an alkaline pH throughout the 72-hour experimental period. BD showed a higher release of calcium ions earlier than did the other materials, also producing higher levels of ion release in most of the experimental periods. This feature could have an effect on previously described positive aspects of BD such as good biocompatibility, bioactivity,³² and biomineralization.³³ Thus, the ability of BD to promote pulp mineralization in shorter periods than the other bioceramic materials has been suggested in an entire human tooth culture model.¹⁰

Among other characteristics, an ideal bioceramic material should be more radiopaque than dentin and tooth surrounding structures. In the current investigation, two methods for evaluation of radiopacity were compared, showing that under the influence of tissue superimposition, bioceramic materials presented significantly higher radiopacity than when they were evaluated by the ISO-recommended method. The tissue simulator block has already been successfully used in studies on the diagnosis of external apical root resorption¹⁶ and in the evaluation of radiopacity of root filling materials.¹⁷,¹⁸ As with the present investigation, previous studies using the same tissue simulator used herein have shown higher radiopacity of endodontic materials than in the ISO-recommended method.¹⁷,¹⁸

Previous studies evaluating the radiopacity of bioceramic materials have used only the ISO-recommended method. In agreement with the current outcomes, Guimarães et al.⁶ showed that MTA-HP meets the criteria recommended by ISO 6876:2012,²¹ presenting similar radiopacity when compared to MTA-A. Note that, in that study, as well as in the other investigations on MTA Angelus radiopacity,¹⁵,³⁴ bismuth oxide was still used as radiopacifier. The current outcomes revealed that calcium tungstate was able to maintain suitable radiopacity of MTA-A in both methodologies used.

Conflicting results have been observed for BD radiopacity in previous investigations, which ranged from suitable¹⁴,³⁵ to inappropriate according to ISO²⁴. The current results show that BD met the ISO criteria and, although it presents lower radiopacity compared to other materials, these differences are probably clinically irrelevant. As a matter of fact, in the present study, dentin presented lower radiopacity than did BD. The tissue simulator method employed herein has allowed evaluating radiopacity closer to what is observed clinically. Therefore, under the influence of tissue superimposition, radiopacity tends to be higher, confirming that BD can be employed in dental practice.

Conclusion

In conclusion, MTA-A, MTA-HP, and BD showed appropriate physicochemical properties and can thus be used in clinical practice.

References

• ¹
  Torabinejad M, Watson TF, Pitt Ford TR. Sealing ability of a mineral trioxide aggregate when used as a root end filling material. J Endod. 1993 Dec;19(12):591–5. https://doi.org/10.1016/S0099-2399(06)80271-2
  » https://doi.org/10.1016/S0099-2399(06)80271-2
• ²
  Ford TR, Torabinejad M, Abedi HR, Bakland LK, Kariyawasam SP. Using mineral trioxide aggregate as a pulp-capping material. J Am Dent Assoc. 1996 Oct;127(10):1491-4. https://doi.org/10.14219/jada.archive.1996.0058
  » https://doi.org/10.14219/jada.archive.1996.0058
• ³
  Shabahang S, Torabinejad M, Boyne PP, Abedi H, McMillan P. A comparative study of root-end induction using osteogenic protein-1, calcium hydroxide, and mineral trioxide aggregate in dogs. J Endod. 1999 Jan;25(1):1-5. https://doi.org/10.1016/S0099-2399(99)80388-4
  » https://doi.org/10.1016/S0099-2399(99)80388-4
• ⁴
  Aeinehchi M, Eslami B, Ghanbariha M, Saffar AS. Mineral trioxide aggregate (MTA) and calcium hydroxide as pulp-capping agents in human teeth: a preliminary report. Int Endod J. 2003 Mar;36(3):225-31. https://doi.org/10.1046/j.1365-2591.2003.00652.x
  » https://doi.org/10.1046/j.1365-2591.2003.00652.x
• ⁵
  Camilleri J, Montesin FE, Brady K, Sweeney R, Curtis RV, Ford TR. The constitution of mineral trioxide aggregate. Dent Mater. 2005 Apr;21(4):297-303. https://doi.org/10.1016/j.dental.2004.05.010
  » https://doi.org/10.1016/j.dental.2004.05.010
• ⁶
  Guimarães BM, Prati C, Duarte MA, Bramante CM, Gandolfi MG. Physicochemical properties of calcium silicate-based formulations MTA Repair HP and MTA Vitalcem. J Appl Oral Sci. 2018 Apr;26(5):e2017115. https://doi.org/10.1590/1678-7757-2017-0115
  » https://doi.org/10.1590/1678-7757-2017-0115
• ⁷
  Marciano MA, Costa RM, Camilleri J, Mondelli RF, Guimarães BM, Duarte MA. Assessment of color stability of white mineral trioxide aggregate angelus and bismuth oxide in contact with tooth structure. J Endod. 2014 Aug;40(8):1235-40. https://doi.org/10.1016/j.joen.2014.01.044
  » https://doi.org/10.1016/j.joen.2014.01.044
• ⁸
  Cavenago BC, Pereira TC, Duarte MA, Ordinola-Zapata R, Marciano MA, Bramante CM, et al. Influence of powder-to-water ratio on radiopacity, setting time, pH, calcium ion release and a micro-CT volumetric solubility of white mineral trioxide aggregate. Int Endod J. 2014 Feb;47(2):120-6. https://doi.org/10.1111/iej.12120
  » https://doi.org/10.1111/iej.12120
• ⁹
  Ferreira CM, Sassone LM, Gonçalves AS, Carvalho JJ, Tomás-Catalá CJ, García-Bernal D, et al. Physicochemical, cytotoxicity and in vivo biocompatibility of a high-plasticity calcium-silicate based material. Sci Rep. 2019 Mar;9(1):3933. https://doi.org/10.1038/s41598-019-40365-4
  » https://doi.org/10.1038/s41598-019-40365-4
• ¹⁰
  Laurent P, Camps J, About I. Biodentine(TM) induces TGF-β1 release from human pulp cells and early dental pulp mineralization. Int Endod J. 2012 May;45(5):439-48. https://doi.org/10.1111/j.1365-2591.2011.01995.x
  » https://doi.org/10.1111/j.1365-2591.2011.01995.x
• ¹¹
  Nielsen MJ, Casey JA, VanderWeele RA, Vandewalle KS. Mechanical properties of new dental pulp-capping materials. Gen Dent. 2016 Jan-Feb;64(1):44-8.
• ¹²
  Asgary S, Parirokh M, Eghbal MJ, Brink F. Chemical differences between white and gray mineral trioxide aggregate. J Endod. 2005 Feb;31(2):101-3. https://doi.org/10.1097/01.DON.0000133156.85164.B2
  » https://doi.org/10.1097/01.DON.0000133156.85164.B2
• ¹³
  Koubi S, Elmerini H, Koubi G, Tassery H, Camps J. Quantitative evaluation by glucose diffusion of microleakage in aged calcium silicate-based open-sandwich restorations. Int J Dent. 2012;2012:105863. https://doi.org/10.1155/2012/105863
  » https://doi.org/10.1155/2012/105863
• ¹⁴
  Camilleri J, Sorrentino F, Damidot D. Investigation of the hydration and bioactivity of radiopacified tricalcium silicate cement, Biodentine and MTA Angelus. Dent Mater. 2013 May;29(5):580-93. https://doi.org/10.1016/j.dental.2013.03.007
  » https://doi.org/10.1016/j.dental.2013.03.007
• ¹⁵
  Tanalp J, Karapınar-Kazandağ M, Dölekoğlu S, Kayahan MB. Comparison of the radiopacities of different root-end filling and repair materials. ScientificWorldJournal. 2013 Oct;2013:594950. https://doi.org/10.1155/2013/594950
  » https://doi.org/10.1155/2013/594950
• ¹⁶
  Gegler A, Fontanella V. In vitro evaluation of a method for obtaining periapical radiographs for diagnosis of external apical root resorption. Eur J Orthod. 2008 Jun;30(3):315-9. https://doi.org/10.1093/ejo/cjm125
  » https://doi.org/10.1093/ejo/cjm125
• ¹⁷
  Malka VB, Hochscheidt GL, Larentis NL, Grecca FS, Fontanella VR, Kopper PM. A new in vitro method to evaluate radio-opacity of endodontic sealers. Dentomaxillofac Radiol. 2015;44(5):20140422. https://doi.org/10.1259/dmfr.20140422
  » https://doi.org/10.1259/dmfr.20140422
• ¹⁸
  Hoppe CB, Baldissera RS, Scarparo RK, et al. A new assessment methodology to evaluate the radiopacity of endodontic filling materials. J Dent Sci. 2013;1:13-7.
• ¹⁹
  Bosso-Martelo R, Guerreiro-Tanomaru JM, Viapiana R, Berbert FL, Duarte MA, Tanomaru-Filho M. Physicochemical properties of calcium silicate cements associated with microparticulate and nanoparticulate radiopacifiers. Clin Oral Investig. 2016 Jan;20(1):83-90. https://doi.org/10.1007/s00784-015-1483-7
  » https://doi.org/10.1007/s00784-015-1483-7
• ²⁰
  International Organization for Standardization. ISO 6876:2012 - Dental root canal sealing materials. Geneva: I International Organization for Standardization; 2012.
• ²¹
  American Dental Association. ANSI/ADA Specification Nº 57 for Endodontic sealing materials. Chicago: ANSI/ADA; 2000.
• ²²
  Carvalho-Júnior JR, Guimarães LF, Correr-Sobrinho L, Pécora JD, Sousa-Neto MD. Evaluation of solubility, disintegration, and dimensional alterations of a glass ionomer root canal sealer. Braz Dent J. 2003;14(2):114-8. https://doi.org/10.1590/S0103-64402003000200008
  » https://doi.org/10.1590/S0103-64402003000200008
• ²³
  Vogel GL, Chow LC, Brown WE. A microanalytical procedure for the determination of calcium, phosphate and fluoride in enamel biopsy samples. Caries Res. 1983;17(1):23-31. https://doi.org/10.1159/000260645
  » https://doi.org/10.1159/000260645
• ²⁴
  Duarte MA, Marciano MA, Vivan RR, Tanomaru Filho M, Tanomaru JM, Camilleri J. Tricalcium silicate-based cements: properties and modifications. Braz Oral Res. 2018 Oct;32 suppl 1:e70. https://doi.org/10.1590/1807-3107bor-2018.vol32.0070
  » https://doi.org/10.1590/1807-3107bor-2018.vol32.0070
• ²⁵
  Kaup M, Schäfer E, Dammaschke T. An in vitro study of different material properties of Biodentine compared to ProRoot MTA. Head Face Med. 2015 May;11(1):16. https://doi.org/10.1186/s13005-015-0074-9
  » https://doi.org/10.1186/s13005-015-0074-9
• ²⁶
  Camilleri J, Pitt Ford TR. Mineral trioxide aggregate: a review of the constituents and biological properties of the material. Int Endod J. 2006 Oct;39(10):747-54. https://doi.org/10.1111/j.1365-2591.2006.01135.x
  » https://doi.org/10.1111/j.1365-2591.2006.01135.x
• ²⁷
  Camilleri J. Evaluation of the physical properties of an endodontic Portland cement incorporating alternative radiopacifiers used as root-end filling material. Int Endod J. 2010 Mar;43(3):231-40. https://doi.org/10.1111/j.1365-2591.2009.01670.x
  » https://doi.org/10.1111/j.1365-2591.2009.01670.x
• ²⁸
  Darvell BW, Wu RC. “MTA”: an hydraulic silicate cement: review update and setting reaction. Dent Mater. 2011 May;27(5):407-22. https://doi.org/10.1016/j.dental.2011.02.001
  » https://doi.org/10.1016/j.dental.2011.02.001
• ²⁹
  Jiménez-Sánchez MD, Segura-Egea JJ, Díaz-Cuenca A. Physicochemical parameters: hydration performance relationship of the new endodontic cement MTA Repair HP. J Clin Exp Dent. 2019 Aug;11(8):e739-44. https://doi.org/10.4317/jced.56013
  » https://doi.org/10.4317/jced.56013
• ³⁰
  Malkondu O, Karapinar Kazandag M. Kazazoglu. A review on Biodentine, a contemporary dentine replacement and repair material. BioMed Res Int. 2014;2014:160951. https://doi.org/10.1155/2014/160951
  » https://doi.org/10.1155/2014/160951
• ³¹
  Bortoluzzi EA, Juárez Broon N, Duarte MAH, Demarchi ACO, Bramante CM. The use of a setting accelerator and its effect on pH and calcium ion release of mineral trioxide aggregate and white Portland cement. J Endod. 2006 Dec;32(12):1194-7. https://doi.org/10.1016/j.joen.2006.07.018
  » https://doi.org/10.1016/j.joen.2006.07.018
• ³²
  Han L, Okiji T. Uptake of calcium and silicon released from calcium silicate-based endodontic materials into root canal dentine. Int Endod J. 2011 Dec;44(12):1081-7. https://doi.org/10.1111/j.1365-2591.2011.01924.x
  » https://doi.org/10.1111/j.1365-2591.2011.01924.x
• ³³
  Zanini M, Sautier JM, Berdal A, Simon S. Biodentine induces immortalized murine pulp cell differentiation into odontoblast-like cells and stimulates biomineralization. J Endod. 2012 Sep;38(9):1220-6. https://doi.org/10.1016/j.joen.2012.04.018
  » https://doi.org/10.1016/j.joen.2012.04.018
• ³⁴
  Marciano MA, Camilleri J, Lucateli RL, Costa RM, Matsumoto MA, Duarte MA. Physical, chemical, and biological properties of white MTA with additions of AlF3. Clin Oral Investig. 2019 Jan;23(1):33-41. https://doi.org/10.1007/s00784-018-2383-4
  » https://doi.org/10.1007/s00784-018-2383-4
• ³⁵
  Grech L, Mallia B, Camilleri J. Investigation of the physical properties of tricalcium silicate cement-based root-end filling materials. Dent Mater. 2013 Feb;29(2):e20-8. https://doi.org/10.1016/j.dental.2012.11.007
  » https://doi.org/10.1016/j.dental.2012.11.007

Publication Dates

• Publication in this collection
  02 May 2022
• Date of issue
  2022

History

• Received
  14 July 2020
• Reviewed
  04 Jan 2021
• Accepted
  22 Mar 2021