Elemental Composition and Dentin Bioactivity at the Interface with AH Plus Bioceramic Sealer: An Energy-Dispersive X-Ray Spectroscopy Study

Abstract

In recent decades, there has been significant growth in research focused on biocompatible materials, particularly in the field of materials science and engineering. The primary advantages of these materials are their biocompatibility, bioactivity, and antibacterial properties. Consequently, there has been a growing utilization of bioceramic sealers in the field of endodontics. This study investigated the amounts of bioactive elements in dentin in contact with the AH Plus^® Bioceramic Sealer (Dentsply, Konstanz, Germany). The results were qualitatively evaluated by examining scanning electron microscopy (SEM) images and elemental mapping and quantitatively by determining element weight (wt%) and atomic (at%) percentages obtained from EDX analysis. The AH Plus^® Bioceramic Sealer demonstrated notable bioactivity through its dynamic contact with dentin at the root level.

1. Introduction

Achieving success in endodontic therapy is contingent upon accurately utilizing devices and materials throughout cleansing and filling the root canal system. The purpose of the obturation phase is to create a completely sealed barrier throughout the endodontic system. This will inhibit the entry of microorganisms into the root canal system via the foramen, coronal, and periapical tissue fluids. Additionally, it will serve as a preventive measure against apical periodontitis lesions.

Globally, fifty percent of adults possess at least one tooth affected by apical periodontitis [1]. Increasing evidence suggests that the bacteremia and low-grade systemic inflammation associated with chronic apical periodontitis may adversely affect general health, perhaps contributing to cardiovascular diseases, adverse pregnancy outcomes, and diabetes, which complicates blood sugar regulation [2]. Moreover, compelling research indicates that effective root canal therapy enhances general health by reducing the inflammatory load [2]. Maintaining proper dental hygiene, mainly through the regular removal of dental plaque, is essential for preventing microbial infiltration that may result in complications like apical periodontitis [3].

Root canal obturation is commonly carried out by employing a core substance, typically gutta-percha, together with an endodontic sealer. Grossman (1981) states that an optimal endodontic sealer must possess several attributes to ensure a successful endodontic treatment [4,5,6]. These include biocompatibility, antibacterial properties, dimensional stability, dentin and core material adherence, radiopacity, and flowability. It is crucial to recognize that, although Grossman’s ideal sealer offers a structure for desirable characteristics [6], no sealer can presently encompass all of these traits. Sealers are often selected by clinicians depending on the individual requirements of each case, taking into account aspects like biocompatibility, handling characteristics, and therapeutic efficacy. Previously, epoxy resin-based sealers were the preferred choice for sealants in endodontics. The interaction between hexamethylene tetramine and bis-phenol resin monomer undergoes ring-opening polymerization, resulting in their solidification. However, not all endodontic sealers are compatible with the tissues at the apex of the tooth [7]. One example is AH26 (Dentsply Sirona, York, PA, USA), which is an epoxy resin sealer that utilizes hexamethylene–tetramine (methenamine) for the process of polymerization [8]. One significant drawback of methenamine is its tendency to emit formaldehyde during solidification. Consequently, dentists tend to favor alternative forms of sealants [9].

In recent decades, there has been substantial growth in study within materials science and engineering, specifically focusing on biocompatible materials, often known as biomaterials, replacing materials with cytotoxic potential [10]. The primary benefits of these materials include their ability to interact well with living organisms, their capacity to promote biological processes, and their strong ability to combat microbial growth [4]. Due to these specific criteria, dentists are progressively utilizing bioceramic sealants. Meanwhile, they do not experience any size-reduction and retain their volume for a prolonged duration [4,5]. Thus, it is feasible to utilize bioceramic sealers in greater quantities without augmenting the quantity of gutta-percha within the root canal. It is advisable to utilize hydraulic calcium silicate-based sealers in conjunction with a single-cone obturation procedure. The gutta-percha cone increases hydraulic pressure in the root canal and pushes the sealer into isthmuses, anomalies, and dentinal tubules [11,12,13]. This obturation technique is readily adaptable, even for doctors with less expertise. Research has demonstrated that bioceramic sealers have a heightened capacity to promote collagen synthesis, hence assisting in tissue regeneration [14].

Moreover, the process of forming crystals in bioceramic sealers such as carbonate apatite (CO₃Ap) is crucial for their bioactivity and their sealing ability in endodontic procedures.

Recently, there has been a development in the field of root canal therapy with the advent of premixed flowable sealers. Unlike other formulations, these materials are pre-prepared and do not require blending, as their solidification process occurs when moisture is exposed [14]. Scientists have documented that those materials containing calcium silicate have a beneficial interaction with the tissues surrounding the apex of a tooth without causing any inflammation or adverse reactions from the body [12,13,14].

The chemical composition of hydraulic calcium silicate-based sealers is broadly consistent among various brands. Tricalcium silicate is the main component responsible for the cementitious properties [15]. Root canal sealers must comply with the specifications stated in ISO 6976:2012 [16].

AH Plus^® Bioceramic Sealer (Dentsply, Konstanz, Germany) is a pre-made sealer primarily consisting of zirconium dioxide (50–70%) as a radiopacifier and tricalcium silicate (10–15%) as a bioactive ingredient. In addition, the producer states that the product contains dimethyl sulfoxide, small amounts of lithium carbonate, and substances used to thicken it. This study aimed to evaluate the bioactivity of AH Plus^® Bioceramic Sealer (Dentsply, Konstanz, Germany) by analyzing the concentrations of bioactive elements in dentin at the interface with the bioceramic sealer. Furthermore, this study can highlight several aspects associated with these sealers that pertain to their performance, efficiency, and bioactive interactions with dentin. Even though bioceramic materials have proven to be biocompatible and capable of forming hydroxyapatite at the dentin-sealer interface, more studies are needed to evaluate their long-term efficacy, particularly regarding their porosity and chemical stability [17,18,19,20,21].

The objective of this study was to evaluate the elemental composition of dentin at the interface with a bioceramic sealer using scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) and to assess the bioactive potential of the constituent elements at the sealer–dentin interface.

2. Materials and Methods

A total of 110 adult incisors (both upper and lower) with a single canal system were extracted for periodontal concerns. The teeth were thoroughly cleaned using ultrasonic technology to remove debris and then placed in a solution containing 0.1% thymol for 3 h. Immediately after extraction, the incisors were decoronated by cutting them 1 mm above the junction between the enamel and cement. Then, an opening was made to access the inside of the tooth. The tooth length was determined using a number 10 ISO hand K-file (Dentsply/Sirona, Switzerland). After that, the tooth was prepared using the TruNatomy system (Dentsply/Sirona, Switzerland) until it reached a foraminal diameter of either 0.25 or 0.35, depending on the specific case.

The teeth were flushed with 20 mL sodium hypochlorite 5.25% (NaOCl) and 5 mL ethylenediaminetetraacetic acid 17% (EDTA), and then dried using sterile paper points (Dentsply/Sirona, Switzerland) and then sealed with Ah Plus^® Bioceramic Sealer (Dentsply, Konstanz, Germany) and TruNatomy Conform Fit gutta-percha points (Dentsply/Sirona, Switzerland) using the hydraulic technique. The roots were placed into plastic containers and embedded into alginate (Henry Schein, Melville, NY, USA). Afterwards, the roots were stored in an incubator (Memmert IN 75 Incubator, Buechenbach, Germany) at 100% humidity and a temperature of 37 °C for 2 weeks. Subsequently, the teeth were placed into blocks made of auto-polymerizing methyl methacrylate acrylic resin.

The roots were horizontally severed at the apical region, specifically 5 mm away from the apex, the samples were taken from the apical and cervical regions. The slices were cut with a microtome (IsoMet Low Speed Precision Cutter, Buehler, Dusseldorf, Germany) at 1 mm thickness, and two slices were cut from each tooth. After that, the samples were dried and sputter-coated with gold. Finally, the surfaces were analyzed with a scanning electron microscope at ×100–×25,000 magnification. Scanning electron microscopy (SEM) was carried out using the Quanta Inspect F50 (FEI Company, Eindhoven, The Netherlands) at a 10 kV and 20 kV acceleration electron voltage. A total of 220 slices from 110 teeth were analyzed using SEM-EDX.

This study utilized a series of SEM images taken at different levels of magnification (ranging from 100× to 25,000×) to examine the detailed structure and the interface between dentin and the sealer. The X-ray energy dispersive spectrometer (EDX) (Thermo Fisher, Eindhoven, The Netherlands) was used in order to determine the elemental distribution at the interface between the dentin and the sealer as well as the elemental distribution of intermediary dentin located at a minimum distance of 50 microns from the dentin in direct contact with the sealer. Measurements were taken in four zones from each specimen, with two from the intermediate dentin level (Area 1) and two from the dentin–sealer interface (Area 2). The results were assessed comprehensively, both qualitatively using SEM pictures and elemental mapping, and quantitatively using element weight (wt%) and atomic (at%) percentages from the EDX study. The particle size was determined using ImageJ 1.52d software (Wayne Rasband, National Institutes of Health, USA) at the intermediate dentin level and at the dentin–sealer interface. The study examined the data using descriptive analysis, calculated the distribution frequencies in percentages, and conducted chi-squared tests to compare proportions. Significance was attributed to p-values less than 0.05. The statistical analyses were conducted using the DATAtab software accessed on 9 September 2024, version (2024) [22].

3. Results

SEM images allow detailed observation of how the endodontic sealant interacts with dentin (Figure 1 and Figure 2).

The images in Figure 1 appear to have a surface with larger particles, indicating a more porous texture.

The images in Figure 2 show a finer and more detailed structure, at a higher magnification.

In order to analyze the results obtained from the SEM examination, the chemical compositions of the samples were determined in the dentin along the interface between the dentin and the filling material, as well as in the surrounding dentin. The weight (weight %) and atomic (atomic %) percentages of carbon, oxygen, phosphorus, magnesium, calcium, and silicon were measured for this specific objective.

Figure 3 is an SEM image (upper incisor) that shows the dentin–bioceramic sealer contact in more detail. Two important areas are highlighted: selected area 1 at the level of the intermediate dentin and selective area 2 at the level of the dentin–bioceramic sealer interface.

Table 1 and Figure 4 provide information about the chemical makeup of a sample from an upper incisor. This sample is likely associated with the SEM pictures of the interface between dentin and a bioceramic sealer in Area 2. The dataset reveals a high oxygen, phosphorus, and calcium concentration, suggesting a significant abundance of phosphate molecules, specifically hydroxyapatite. This composition exemplifies the characteristics commonly seen in bioceramic materials utilized in dental applications. Its purpose is to adhere to dentin and effectively facilitate biological integration. A relatively low carbon content indicates that the sample preparation was performed effectively, with minimal organic contamination. Sodium and magnesium are present in moderate quantities, potentially added to augment particular characteristics of the substance, such as its mechanical robustness and bioactivity. Minor quantities of silicon are present, potentially influencing the overall characteristics of the bioceramic material.

Table 2 and Figure 5 describe the elemental composition of an upper incisor sample, likely related to the SEM images of the intermediary dentin (Area 1), in the apical region.

The notable occurrence of carbon (C—23.04% weight, 35.23% atomic) may be attributed to organic components present in the dentin. Phosphorus and calcium, with a weight percentage of 12.76% and 21.80%, respectively, and an atomic percentage of 7.57% and 9.99%, respectively, are essential components of hydroxyapatite (Ca₅(PO₄)₃(OH)₂), the main mineral found in dentin. Their existence serves as evidence of the mineral composition of dentin. Sodium, magnesium, and silicon (Na—1.91% by weight, 1.52% by atomic percentage; Mg—1.06% by weight, 0.80% by atomic percentage; Si—0.80% by weight, 0.53% by atomic percentage) could potentially be present as trace elements in the bioceramic sealer.

In Figure 6, a scanning electron microscope (SEM) picture of an inferior incisor dentin–filler interface is presented, displaying two selected locations for study.

Figure 6 displays the SEM image of the dentin interface with the filling material in an apical slice of an inferior incisor. The image highlights two specific locations that have been chosen for investigation. Area 1 was chosen at the intermediate dentin level, while Area 2 at dentin–bioceramic sealer interface (the dentin region).

Table 3 and Figure 7 provide an account of the chemical makeup of a sample taken from the interface between the dentin and bioceramic sealer in an inferior incisor, at an apical level (Area 2). The dataset once again indicates a significant presence of phosphorus (16.57%) and calcium (24.38%).

Table 4 and Figure 8 provide an account of the elemental makeup of a sample from the outer layer of dentin (Area 1) of an inferior incisor.

The EDX elemental mapping revealed different elemental compositions (Figure 9 and Figure 10).

Table 5 presents the comparative distribution of bioactive elements at various regions (dentin–sealer interface and intermediate dentin) and levels (coronal and apical).

Table 6 presents the mean weight percentages (wt%) of bioactive elements at the dentin–sealer interface (DSI) and intermediate dentin (ID) for all 220 slices from the 110 teeth. This comparison assesses the influence of the bioceramic sealer on the elemental composition at the immediate interface (DSI) compared to the adjacent, unaffected dentin region (ID) to evaluate the potential bioactivity and diffusion of elements from the sealer into the surrounding dentin.

4. Discussion

The investigation revealed that the concentration of calcium ions was more significant at the interface with the bioceramic sealer compared to the intermediate dentin. This phenomenon is because calcium silicate in bioceramic sealers undergoes a reaction with dentin fluids, forming calcium hydroxide. This undergoes a transformation into hydroxyapatite, a naturally occurring calcium apatite mineral found in bone and dental tissues. Hydroxyapatite forms strong connections with the sealer, enhancing the seal and promoting the restoration of minerals in the dentin. Additionally, calcium ions have a role in the recovery of periapical tissues by promoting the differentiation and proliferation of odontoblast-like cells and other cells involved in the healing process [23]. The release of calcium ions from sealers creates a strong chemical connection and improves bioactivity by precipitating an apatite-like layer on the dentin wall [24]. Furthermore, calcium ions may assist in regenerating periapical tissues [25].

Research on the effectiveness of sealing in various clinical conditions has shown that the sealing ability of root canals can vary depending on the obturation technique, and the long-term impact of bioceramic sealers on the healing of periapical lesions is still under investigation [18,19]. It has been found that the migration of chemical elements at the sealer–dentin interface, especially silicon, is critical for the material’s bioactivity. However, there is variability in these interactions depending on the sealer’s composition and clinical conditions [20,21]. In our study, the amount of silicon more than doubled at the dentin–sealer interface compared with intermediate dentin area, with the highest level being found in the coronal sections. Badawy et al.’s research found the same results, with the Si concentration being higher along the interface between the dentin and the bioceramic sealer and lower in the surrounding dentin [26].

This study detected the highest phosphorus concentration at the dentin–sealer interface in the apical region, highlighting the sealer’s bioactivity and its potential to enhance mineralization in this crucial area for tissue regeneration. Conversely, the lowest level was observed in the intermediate dentin coronally. Furthermore, in the study of Tamer et al., about the composition of three sealers, the AH Plus Bioceramic Sealer was found to have a mass percentage of 12% P in an EDX analysis [27]. The study conducted by Han et al. emphasizes the same concept, as they found that bioceramic sealers produced phosphorus (P) and calcium (Ca) ions, which in turn facilitated the absorption of calcium and silicon (Si) into the dentine of human root canals, demonstrating bioactivity. Ca and Si uptake by intertubular dentine can indicate a material’s bioactivity [28]. The inclusion of silicon may have biological significance since it promotes the process of dentine remineralization in a laboratory setting [29]. This underscores the potential of silicon in enhancing the bioactivity of materials used in dental applications. The Si content in the sealer is well established, as confirmed by the technical data sheet of the material and in the study of Tamer at al., where it was found in an EDX analysis to be at a mass percentage of 2.25% [27].

The carbon concentration in the intermediate dentin was four times more than that in the dentin near the sealer interface because of the preservation of its biological matrix, mainly collagen, which has a high carbon content. Bioceramic sealers promote mineralization, forming new mineral deposits in dentin, such as hydroxyapatite. This process also enhances the proportion of inorganic substances compared to organic material, decreasing carbon levels near the point of contact with the sealer [30].

The oxygen content was slightly elevated at the dentin from the sealer interface, likely due to the metabolic events that occur during and after their application. Increased oxygen levels enhance the healing processes essential for the success of root canal treatments. Ah Plus Bioceramic sealer comprises calcium silicate-based compounds interacting with dentin fluids, forming calcium hydroxide. This process produces oxygen as a result of the chemical reactions that occur during the formation of hydroxyapatite. The elevated oxygen levels in this region could indicate significant biochemical processes occurring at the interface [31].

The concentration of the element Mg near the contact was higher than in the intermediate dentin. This could be possible because EDTA firmly attaches to bivalent ions, including magnesium and calcium. EDTA can extract considerable magnesium from the root dentin based on the solution’s concentration and application length [32].

The boundary between dentin and a bioceramic sealer exhibited elevated sodium (Na) levels, likely resulting from the irrigation of teeth with sodium hypochlorite (NaOCl) during chemo-mechanical therapy. If sodium is present in the dentinal tubules or on the dentin surface when the sealer is applied, it may result in elevated sodium concentrations at the interface.

This study’s limitations may be due to the absence of ex vivo experiments concerning the sealer utilized in this laboratory-based research, and the lack of a control group. An in vivo setting is necessary for relevant answers to the questions we raised. Subsequent research may expand upon our study to develop an ex vivo root canal model for assessing the physical, chemical, and antibacterial properties of sealants. The utilization of an ex vivo model would substantially enhance our ability to draw clinical findings. The carbon dioxide present in vivo causes the creation of calcium carbonate rather than the hydroxyapatite indicated in vitro research [33], and the material’s in vitro evaluation could affect the study’s relevance to actual clinical conditions [33]. Using energy-dispersive X-ray spectroscopy (EDX) provides valuable insights into the elemental compositions of root canal sealers and their potential interactions with dentin. While EDX is effective in quantifying elemental composition and understanding material distribution at the interface, it has limited capacity to directly assess biological characteristics or the effects of specific constituent elements.

Additional research included in the study by Estivalet et al. has also documented these mineralization processes. The research indicates the possible bioactivity of root canal sealers based on bioceramics [34]. Furthermore, using premixed bioceramic materials can help maintain the vitality of the pulp due to the dentinogenesis process and enhance the resistance to fractures in the radicular wall [35]. In the long run, the treatments’ durability relies not only on the excellence of endodontic treatment but also on the excellence of coronal adhesive restorations, achieved by establishing a seamless connection and ensuring proper marginal fit [36] and on the experience and preferences of the dentists regarding adhesive techniques [37].

5. Conclusions

This study evaluated the elemental composition of dentin at the dentin–sealer interface (DSI) and intermediate dentin (ID) using energy-dispersive X-ray spectroscopy (EDX). The findings revealed distinct elemental distributions, with higher concentrations of bioactive elements such as calcium, phosphorus, and silicon at the DSI, suggesting their migration from the bioceramic sealer. This highlights the potential of bioceramic sealers to enhance the bioactivity of the dentin interface, promoting hydroxyapatite formation and improving the sealing and integration capabilities of the material.

Although EDX analysis effectively quantified elemental composition, its limitations in assessing biological effects or precise chemical interactions must be acknowledged. Future studies should include complementary techniques, such as XPS or FTIR, to provide a deeper understanding of these interactions.

These results support the use of bioceramic sealers in root canal therapy, emphasizing their role in improving long-term clinical outcomes through enhanced material–dentin interactions.

Author Contributions

Conceptualization, D.M., I.V. and M.-M.M.; methodology, O.R.C.; software, A.H.S.; validation, C.C., D.E.P. and R.F.; formal analysis, R.A.P.; investigation, D.M., I.V. and I.O.; resources M.-M.M., D.M., D.E.P., R.F., A.H.S., C.C., E.V. and I.O.; data curation, O.R.C.; writing—original draft preparation, D.M. and I.V.; writing—review and editing, R.A.P.; visualization, I.O. and I.-C.E.; supervision, I.-C.E.; project administration, M.-M.M. and E.V. All authors have read and agreed to the published version of the manuscript.

Institutional Review Board Statement

This study was conducted by the Declaration of Helsinki. The study has been approved by the Ethics Committee of Victor Babes University of Medicine and Pharmacy in Timisoara, Romania, number 75/02.10.2023.

Informed Consent Statement

Informed consent was obtained from all subjects involved in the study. Written informed consent has been obtained from the patients to publish this paper.

Data Availability Statement

The data presented in this study are available upon request from the corresponding author. The data are not publicly available due to privacy and ethical reasons.

Conflicts of Interest

The authors declare no conflicts of interest.

Footnotes

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Figures and Tables

Table 1

Chemical analysis of an upper incisor for Selected Area 2, at the apical level.

Element	Weight %	Atomic %	Net Int.	Error %	Kratio
C K	5.46	9.59	0.34	36.45	0.01
O K	43.96	57.93	4.55	12.14	0.06
NaK	4.89	4.49	1.35	15.33	0.01
MgK	3.37	2.92	1.82	13.72	0.01
SiK	1.02	0.77	1.12	19.95	0.01
P K	16.62	11.32	19.69	5.93	0.10
CaK	24.68	12.98	28.09	3.27	0.21

Table 2

Chemical analysis of an upper incisor for Selected Area 1, at the apical level.

Element	Weight %	Atomic %	Net Int.	Error %	Kratio
C	23.04	35.23	2.25	14.65	0.06
O	38.64	44.36	4.38	12.97	0.07
Na	1.91	1.52	0.54	27.10	0.01
Mg	1.06	0.80	0.49	30.29	0.01
Si	0.80	0.53	0.45	34.11	0.01
P	12.76	7.57	5.99	5.56	0.10
Ca	21.80	9.99	4.52	7.28	0.19

Table 3

Chemical analysis of an upper incisor for Selected Area 2, at the level of the dentin–bioceramic sealer interface, at the apical region.

Element	Weight %	Atomic %	Net Int.	Error %	Kratio
C K	4.15	8.12	2.01	15.17	0.04
O K	31.07	45.66	7.26	11.96	0.09
NaK	4.91	5.02	1.05	17.91	0.01
MgK	3.10	3.00	0.60	26.20	0.01
SiK	1.91	1.06.	0.33	23.55	0.00
P K	25.6	19.44	7.63	5.45	0.10
CaK	29.26	17.70	5.69	6.44	0.19

Table 4

Chemical analysis of an inferior incisor for Selected Area 1, at the intermediate dentin level from the apical region.

Element	Weight %	Atomic %	Net Int.	Error %	Kratio
C K	6.97	11.98	0.38	42.87	0.02
O K	44.89	57.96	3.91	12.92	0.06
NaK	4.91	4.41	1.13	17.72	0.01
MgK	2.84	2.41	1.28	17.11	0.01
P K	16.00	10.67	16.38	6.33	0.10
CaK	23.71	12.57	23.58	3.62	0.21
Si K	0.68	0.45	0.81	19.01	0.01

Table 5

The weight percentage (wt%) of bioactive components in dentin, at dentin–sealer interface area and in intermediate dentin, at both levels: apical and coronal.

	A			C
Element	DSI	ID	p Value	DSI	ID	p Value
C	4.71 ± 0.5	23.15 ± 0.3	≤0.05 *	7.73 ± 0.3	27.31 ± 0.4	≤0.05 *
O	33.15 ± 0.7	36.12 ± 0.8	≤0.05 *	37.23 ± 1.0	33.66 ± 1.2	≤0.05 *
Na	4.38 ± 0.0	1.98 ± 0.0	≤0.05 *	6.12 ± 0.1	2.50 ± 0.0	≤0.05 *
Mg	3.35 ± 0.1	0.98 ± 0.1	≤0.05 *	4.27 ± 0.2	1.16 ± 0.0	≤0.05 *
Si	1.87 ± 0.1	0.76 ± 0.2	≤0.05 *	2.26 ± 0.1	0.90 ± 0.1	≤0.05 *
P	23.47 ± 0.4	16.91 ± 0.1	≤0.05 *	14.71 ± 0.3	10.33 ± 0.3	≤0.05 *
Ca	29.07 ± 0.5	20.1 ± 0.6	≤0.05 *	27.69 ± 0.4	24.14 ± 0.5	≤0.05 *

DSI, dentin–sealer interface, ID, intermediate dentin, A, apical level, C, coronal level, chi-square test, * statistically significant differences between the w% of elements at various root levels p < 0.05.

Table 6

The weight percentage (wt%) of bioactive components of dentin at the sealer–dentin interface and of intermediate dentine at both levels.

	DSI	ID
Element	Weight %	Weight %	p Value
C	6.22 ± 0.3	25.23 ± 0.2	≤0.05 *
O	35.19 ± 0.4	32.75 ± 0.3	≤0.05 *
Na	5.25 ± 0.1	2.24 ± 0.0	≤0.05 *
Mg	3.81 ± 0.2	1.07 ± 0.1	≤0.05 *
Si	2.06 ± 0.1	0.83 ± 0.0	≤0.05 *
P	19.09 ± 0.3	12.76 ± 0.3	≤0.05 *
Ca	28.38 ± 0.4	25.12 ± 0.3	≤0.05 *

(*) DSI, dentin–sealer interface, ID, intermediate dentin, chi-square test, statistically significant differences p < 0.05.

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