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Received: 11 August 2021 | Revised: 14 August 2022 | Accepted: 16 August 2022

DOI: 10.1002/cre2.665

ORIGINAL ARTICLE

Evaluating the shear bond strength and remineralization effect


of calcium silicate‐based and conventional self‐adhesive resin
cements to caries‐affected dentin

Maryam S. Tavangar1 | Ayda Safarpour2 | Arefeh Torabi Parizi3 |


Fereshteh Shafiei1

1
Department of Operative Dentistry, Oral and
Dental Disease Research Center, School of Abstract
Dentistry, Shiraz University of Medical
Objective: Given the importance of preserving caries‐affected dentin (CAD) in
Sciences, Shiraz, Iran
2
Students' Research Committee, School of
conservative dentistry, the shear bond strength (SBS) of different resin cements to
Dentistry, Shiraz University of Medical CAD has been investigated. Here, we aimed to compare the SBS and remineralizing
Sciences, Shiraz, Iran
effect of a calcium silicate (TheraCem) and conventional self‐adhesive cement
3
Department of Operative Dentistry, School
of Dentistry, Shiraz University of Medical (Panavia SA) on the SBS of CAD.
Sciences, Shiraz, Iran Materials and Methods: Forty‐eight extracted third molars (24 sound and 24 CAD)
were used. In each group, 12 teeth were prepared for bonding to TheraCem or
Correspondence
Fereshteh Shafiei, Department of Operative Panavia SA. After removal of the enamel and caries, resin composite cylinders were
Dentistry, Oral and Dental Disease Research
luted on the prepared dentin. After 28 days of storage in the artificial saliva, SBS was
Center, Shiraz University of Medical Sciences,
Ghasrdasht St, Shiraz 71345‐1836, Iran. measured and the failure mode analysis was investigated. The images of fractured
Email: shafieif@sums.ac.ir
sections were analyzed using scanning electron microscopy and energy‐dispersive
Funding information X‐ray to evaluate the Ca/P weight ratio.
The vice‐chancellery of Shiraz University of Results: SBS of CAD and sound dentin was not different when cemented with
Medical Sciences, Grant/Award Number:
21193
TheraCem (9.56 ± 4.51 vs. 9.17 ± 2.76, p = .806), but the CAD showed significantly
lower SBS to Panavia SA (9.4 ± 2.36 vs. 7.39 ± 2.18, p = .015). The Ca/P ratio in CAD
was significantly higher when bonded to both TheraCem and Panavia‐SA than that of
the controls (p = .001); however, this ratio was not different for those bonded to
TheraCem compared to Panavia SA.
Conclusions: Based on our results, TheraCem as a calcium silicate cement shows
better SBS to attach the restoration to CAD as compared to Panavia SA. Obliteration
and mineralization of the dentinal tubules in TheraCem were also higher than in
Panavia SA. However, their ability to improve the amount of the Ca/P ratio in CAD
was similar.

KEYWORDS
calcium silicate, caries affected dentin, remineralization, self‐adhesive resin cement, shear bond
strength

This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium,
provided the original work is properly cited.
© 2022 The Authors. Clinical and Experimental Dental Research published by John Wiley & Sons Ltd.

1630 | wileyonlinelibrary.com/journal/cre2 Clin Exp Dent Res. 2022;8:1630–1637.


TAVANGAR ET AL. | 1631

1 | INTRODUCTION been investigated. To the best of our knowledge, there are no studies
to investigate the bond strength of TheraCem to CAD and its
Carious dentin consists of two layers. The outer layer known as remineralization effect on this substrate. Accordingly, this study
caries‐infected dentin (CID) is highly demineralized, is physiologically aimed to investigate the SBS strength of TheraCem to CAD in
not remineralizable, and contains irreversibly denatured collagen comparison with Panavia SA, as a conventional resin cement. Also,
fibrils with the disappearance of cross‐linkages. On the other hand, the mineral content of the bonded dentin would be evaluated as it is
the inner layer or caries‐affected dentin (CAD) is partially deminer- claimed that TheraCem can release calcium monophosphate ions. The
alized and physiologically remineralizable (Kuboki et al., 1977). High null hypothesis of this study is that the remineralization effect
porosity, partially demineralized dentin, exposure of collagen fibers and the bond strength of both conventional and Ca‐silicate‐based
along with a decrease in the surface energy, and the reduction in resin cements on sound and CAD are not different.
intermolecular cross‐links of the collagen are the alterations shown in
this tissue (Taniguchi et al., 2009). Meanwhile, there is evidence
indicating that structural changes in CAD are reversible (Meraji et al., 2 | METHODS
2018). Consequently, minimally invasive restorative dentistry is
recommended to preserve the CAD to protect the tooth structure 2.1 | Materials
and vitality of the pulp in direct and indirect restorations (Elsharkawy,
2018; Pintado‐Palomino et al., 2019). However, because of the Table 1 presents the main materials used in the study.
chemical and mechanical alterations in CAD, such as a thicker and
irregular smear layer with fibril‐like structures, and the presence of
narrow and occlude dentinal tubules (Meraji et al., 2018; Pintado‐ 2.2 | Specimen preparation
Palomino et al., 2019; Taniguchi et al., 2009), bonding to CAD is
challenging. Several studies indicated that CAD showed lower bond Forty‐eight extracted third molars, 24 sound and 24 with occlusal pit
strength compared to sound dentin (Elsharkawy, 2018; Meraji et al., and fissure caries, that were extracted for definite clinical reasons
2018; Pintado‐Palomino et al., 2019). (nonresearch purposes), such as caries, orthodontic purposes, and
The type of adhesive and cement is a determinant factor in the periodontal diseases, were used in this study. The teeth with cracks,
amount of bond strength to CAD (Palma‐Dibb et al., 2003). Currently, severe caries, and previous treatment with chemical agents were
the use of bioactive materials such as glass ionomer cements, excluded from the study.
composite resins, and adhesives containing bioactive materials is The teeth were cleaned with fluoride‐free prophylaxis paste
recommended to restore CAD. These materials release ions (e.g., (Protec prophylaxis paste, Medicept) and then kept in 4% thymol
calcium and phosphate) that induce mineral deposition and reminer- solution (Sigma‐Aldrich) at room temperature for 2–3 weeks before
alization of CAD and improve mechanical strength, thus extending the examination. The enamel of the occlusal surface was removed
the durability of the resin‐dentin bond (Elsharkawy, 2018; Alrahlah, using a diamond disc (Drux) and then ground flat with 600‐grit silicon
2018; Profeta et al., 2012, 2013; Sauro et al., 2012). In addition, these carbide abrasive paper (Extec Corp.) for 1 min under running water to
materials reduce biofilm penetration into the marginal gaps because create a uniform smear layer.
of the toxic effect of fluoride, calcium, and phosphate ions. For the teeth affected by caries, the dentin was removed using a
Self‐adhesive resin cements are now very popular among diamond disc (Drux) until the CAD remained. To detect the CAD, the
dentists as they can provide a reliable bond to the dental structures exposed dentin was examined visually and tactility. Surfaces with
while eliminating the etching procedure and need for bonding discolored dentin and resistance to the excavator were considered
application (Mahrous et al., 2020). TheraCem (Bisco) and Panavia CAD. This diagnosis was confirmed by caries detector solution
SA luting plus (Kuraray) are self‐adhesive resin cements containing (Kuraray Co.) applied on the dentin surface following the manufac-
methacryloxydecyl‐dihydrogen‐phosphate (MDP), as an acidic mono- turer's instructions by the second operator (restorative specialist).
mer, to provide superior hydrolytic stability. Panavia SA luting The teeth were ground until the bright pigmentation of the CID was
cements contain silane coupling agents to provide effective bonding removed, and the CAD remained. Then, the samples were mounted
ability, particularly to ceramic surfaces (Yoshihara et al., 2020). using polyethylene mold with self‐cured acrylic resin (Acropars,
TheraCem, as a newly introduced calcium silicate cement, showed an Marlik Co.) (Supporting Information 1).
ability to form crystalline calcium hydroxide, which may improve the
mechanical bond between these cements and dentin (Meraji et al.,
2018). It has the ability to release fluoride and calcium ions, 2.3 | Restorative procedures
contributing to the remineralization of the tooth mineral structures.
Thus, it is suggested as a bioactive material (Van Landuyt et al., 2007; In both sound and affected groups, the teeth were divided
Mahrous et al., 2020; Yoshihara et al., 2010). randomly into two groups (n = 12). One group was prepared for
Given the importance of preserving CAD in conservative bonding to Theracem (Bisco) and the other one was for bonding
dentistry, the bond strength of different resin cements to CAD has to Panavia SA (Kuraray), according to the manufacturer's
1632 | TAVANGAR ET AL.

TABLE 1 Materials used in the study

Material Type Ingredients Steps of application Manufacturer

TheraCem Self‐adhesive Base: Calcium base filler, glass filler, dimethacrylates, (1) Preparation procedure: Bisco
resin ytterbium fluoride, initiator, amorphous silica ̶ Clean the surface with water. Rinse
cement thoroughly
Catalyst: Glass filler, methacryloyloxydecyl‐
̶ Dry the surface using a strong
dihydrogen‐phosphate (MDP), amorphous silica
stream of air for 3–5 s
(2) Mixing procedure:
̶ Dispense a small amount of material
onto a mixing pad to eliminate any
voids in each chamber of the dual
syringe
̶ Attach a mixing tip to the dual‐
syringe
̶ Pressing the plunger will mix and
dispense the material
(3) Cementation procedure:
̶ Apply cement to the tooth
preparation
̶ Remove any excess cement (light
cure the margins 2–3 s)
̶ Final cure (light cure 20–30 s)

Panavia SA Self‐adhesive Paste A: MDP, Bisphenol A diglycidylmethacrylate (1) Preparation procedure: Kuraray
luting plus resin (Bis‐GMA), triethyleneglycol dimethacrylate ̶ Clean the surface with water
cement (TEGDMA), hydrophobic aromatic dimethacrylate, ̶ Dry the surface
2‐hydroxymethacrylate (HEMA), silanated barium (2) Mixing procedure:
glass filler, Silanated colloidal silica, dl‐ ̶ Dispense an equal amount of paste
camphorquinone, peroxide, catalysts, pigments A and B
̶ Mix for 10 s
Paste B: Hydrophobic aromatic dimethacrylate,
(3) Cementation procedure:
hydrophobic aliphatic dimethacrylate, silanated
̶ Apply cement to the tooth
barium glass filler, surface‐treated sodium
preparation
fluoride, accelerators, pigments
̶ Remove any excess cement (light
cure the margins 2–5 s)
̶ Final cure (light cure 10 s)

instructions. The occlusal surface of all samples was rinsed with 2.4 | SBS
distilled water and air‐dried gently before the application of the
cement. Resin composite (FiltekTM Z250, 3M ESPE) cylinders After the initial setting of cement according to the manufacturer's
were fabricated in the polyethylene mold with a dimension of instructions, the molds were removed, and the samples were
4 mm in diameter and 2 mm in length and polymerized using a stored in artificial saliva (NikCeram Razi corp.) in an incubator
light‐emitting diode (LED) unit (LED.F; Woodpecker) with a (Cooled Incubator NUVE ES 250) at 37°C for 28 days, which was
standard method. The blocks were luted on the prepared dentin changed every day (Shaik et al., 2017). To avoid bias in data
with each cement. Subsequently, the excess resin cement around collection, we considered blinding during testing the specimens.
the composite block was removed carefully with a disposable Shear bond testing was performed using a universal testing
brush, and the cement was photopolymerized with the LED light machine (Instron, Z020; Zwick Roell). The samples were placed in a
cure unit, according to the manufacturer's instructions (Table 1). jig, and the force was applied to each specimen parallel to the bonded
While the cement was becoming polymerized, constant pressure interface at a crosshead speed of 1 mm/min until failure occurred.
was applied simultaneously as the static loading to the cementa- The SBS was calculated using the software TestXpert II (Zwick Roell).
tion mold for 5 min.
After performing the restorative procedure, due to the claimed
ability of Ca‐silicate‐based cement (TheraCem) to release calcium 2.5 | Failure mode analysis
monophosphate ions, all the tests including shear bond strength
(SBS), evaluation of the mineral content of the bonded dentin using The debonded surface of the samples was evaluated for failure mode
the energy‐dispersive X‐ray (EDX) method, and scanning electron analysis under ×10 magnification and categorized into three modes:
microscopy (SEM) analysis were done after 4 weeks of aging in Mode 1: Adhesive failure that occurred at the filling material and
artificial saliva. dentine interface
TAVANGAR ET AL. | 1633

Mode 2: Cohesive failure within the filling material


Mode 3: Mixed failure mode (both adhesive and cohesive failures).

2.6 | SEM

The images of the fractured sections of three samples from each


group were examined using an SEM (TESCAN‐Vega 3; TESCAN) at
15 kV and with magnifications of ×500 and ×3500. To prepare the
samples, we dried them in a desiccator and vacuum‐coated them with
approximately 10 nm thickness of gold.

2.7 | EDX analysis


F I G U R E 1 Shear bond strengths of different groups (MPa). The
groups with a significant difference are marked with an asterisk.
Seven samples of each group were sectioned perpendicularly to the
bonded interface using a diamond disc (Drux), as near as possible to
the center of the cylinder. Furthermore, two groups of uncemented
TABLE 2 Specimen numbers of different failure modes for each
sound and CAD as the control groups were also sectioned. Then, all
group
the sections were polished with abrasive discs (Extec Corp.), cleaned
with distilled water, and dried after each polishing step. These Failure mode
Material Dentin substrate Cohesive Mixed Adhesive
samples were prepared similarly to those used for the SEM and
TheraCem Caries affected dentin 0 9 3
examined with the same machine equipped with an EDX spectrome-
ter at 20 kV. The mineral content of intertubular space, just under the Sound dentin 2 9 1
restoration–dentin interface, was measured. Panavia SA Caries affected dentin 0 7 5
luting plus
Sound dentin 0 10 2

2.8 | Statistical analysis

Data are represented as mean ± SD. SPSS software version 22 (SPSS Inc.) failure was only recorded for sound dentin specimens bonded to
was used to analyze the data using an Independent sample t‐test for TheraCem. The most adhesive failure was found for CAD bonded to
comparisons between the cements or dentin substrate. Also, one‐ Panavia SA (Supporting Information: Figure 2).
way analysis of variance was used for the comparison of EDX in the three
groups. The values lower than .05 were considered statistically significant.
3.3 | SEM

3 | RESULTS In the SEM evaluations in lower magnifications, in the CAD samples


that were bonded to Panavia SA, the dentin surfaces showed small
3.1 | SBS areas of covering with few islands on the surface. However,
TheraCem spread more homogenously over the CAD surface and
A comparison of SBS of sound and CAD to Panavia SA and TheraCem with more islands of cement distributed over the remaining area.
showed no difference (p = .99 and .47 to sound and CAD, SEM images revealed depositions on the treated dentinal
respectively). While for TheraCem‐bonded specimens, there was no tubule openings in all groups. Complete obliteration and deposition
significant difference between the two groups of sound dentin and of minerals in dentinal tubule opening in the samples bonded to
CAD (p = .806), in Panavia SA‐bonded specimens, the CAD groups TheraCem were more frequently observed than those bonded to
showed significantly lower bond strength compared to sound dentin Panavia SA, particularly in the CAD surface. Figure 2 shows the
(p = .015, Figure 1). results of SEM imaging.

3.2 | Failure mode analysis 3.4 | EDX analysis

The modes of failure distributions are represented in Table 2. In all Table 3 displays the means and standard deviations for the calcium/
groups, the frequent failure mode was a mixed failure. The cohesive phosphate weight ratio of SD and CAD bonded to both TheraCem
1634 | TAVANGAR ET AL.

F I G U R E 2 Scanning electron microscope examinations: (a) sound dentin bonded to the Panavia SA. (b) Caries affected dentin (CAD) to the
Panavia SA. (c) Sound dentin bonded to the TheraCem. (d) CAD bonded to TheraCem.

TABLE 3 Average of the Ca/P weight ratio Energy dispersive spectroscopic plots of two test materials and

Substrate the control group in sound and CAD are shown in Figure 3. In SEM
images, the intertubular area, which was investigated by EDX
Caries affected
Materials Sound dentin dentin p Value analysis, was defined (Figure 3). The EDX analysis for all groups
A C (TheraCem, Panavia SA, control) showed strong peaks of calcium and
TheraCem 2.39 ± 0.03 2.28 ± 0.29 .29
phosphate. In addition, the highest peak of oxygen and silica among
Panavia SA 2.22 ± 0.16B 2.19 ± 0.19C .67
all groups was noticed for CAD specimens bonded to TheraCem.
luting plus
Furthermore, CAD specimens bonded to TheraCem showed a
Control 2.40 ± 0.10A 1.60 ± 0.06D .001 stronger peak of aluminum than all other groups.
P value 0.007 0.001

Note: Data are represented as mean ± SD. In each column, similar


superscript letters indicate no significant difference between the two 4 | D IS CU SS IO N
items.
In the present study, we evaluated the SBS of a calcium silicate‐based
resin cement (TheraCem) and the conventional self‐adhesive resin
and Panavia SA resin cements and two groups without any cement (Panavia SA) to the sound and CAD. Here, we noticed that
cementation as the positive and negative control. TheraCem shows a similar SBS to both CAD and sound dentine, while
In CAD, EDX analysis showed that the Ca/P weight ratio was Panavia SA cannot. It also shows a less adhesive failure mode.
significantly higher when bonded to both Panavia SA and TheraCem Consequently, TheraCem may be more effective for restorations on CAD.
than that of negative control (p = .001). The mineral content of CAD The results from previous studies indicate that the SBS of various
samples bonded to TheraCem was not significantly different from types of cement to CAD and sound may be dependent on the material.
those bonded to Panavia SA. Suzuki et al. in an investigation on etch and rinse (RelyX ARC), self‐etch
TAVANGAR ET AL. | 1635

F I G U R E 3 Energy dispersive spectroscopy plots of the control group and the test materials accompanied by SEM micrographs of the
intertubular space at the site where the EDX analysis was performed are marked by rectangles. CAD, caries affected dentin; EDX, energy‐
dispersive X‐ray; P, Panavia, SEM, scanning electron microscope; SD, sound dentin; Th, TheraCem.

(Panavia F), and self‐adhesive (RelyX Unicem) resin cements showed that durable chemical bond to hydroxyapatite (Yaguchi., 2017). In addition
there was not a significant difference between the microtensile bond to the acidic monomers, there are other components in TheraCem
strength of these cements to CAD and sound dentin in each group that are key to its bonding capability. Active ingredients such as
(Suzuki et al., 2013). In another study, Czarnecka et al. showed that the calcium and phosphate incorporated in this cement can ionically
SBS of automixed GIC to the sound dentin was not significantly different interact with hydroxyapatite (Piwowarczyk et al., 2004). There are
from CAD, while the SBS of the hand‐mixed GIC to the sound dentin was some evidence that showed that adhesive resins with added calcium
higher than CAD (Czarnecka et al., 2007). Choi et al. reported that the and phosphate ions can act as an ion reservoir that facilitates the
microtensile bond strengths of conventional GIC and RMGIC to CAD remineralization of the tooth surfaces and may enhance the SBS to
were significantly lower than those of the sound dentin (Choi et al., 2006). tooth structures (Ranjkesh et al., 2016; Shadman et al., 2015). Some
Our findings indicating that the SBS of TheraCem to the sound and CAD previous studies have clarified that CAD may exhibit a lower bond
is similar and that for Panavia SA is lower to CAD provide another strength to the cements and this has contributed to the partial
evidence that the SBS of some materials depends on their biochemical demineralization in this tissue (Meraji et al., 2018). Consequently, the
properties. remineralization effect of TheraCem may explain its better SBS to
The results from the present study, depicting a similar SBS to CAD as compared to Panavia SA.
sound dentin for both TheraCem and Panavia SA cement, may be In our study, SEM images showed obliteration and mineralization
explained by the presence of the same functional monomer (MDP), of the dentinal tubules in TheraCem, which were more frequent than
which makes their stable bond to dentin surfaces. It is established in Panavia SA. In addition to the probability of mineral deposition in
that the adhesion of resin cement to teeth depends on their the dentinal tubules, more alkaline properties of these cements,
micromechanical interlocking and chemical adhesion to the tooth compared to other self‐adhesive cements, may explain less dissolu-
substrate (Mahrous et al., 2020). It was reported that the type of the tion of the smear layer and probably keep more smear plugs within
functional monomer in adhesives may play a major role in providing a the opened dentinal tubules (Miletic, 2018; Yaguchi, 2017).
1636 | TAVANGAR ET AL.

In this study, the mixed failure mode was predominant in all revised the manuscript. All authors gave their final approval and
groups. The cohesive failure was only recorded for sound dentin agree to be accountable for all aspects of the work.
bonded to TheraCem, which may be related to the low resistance of
the tested material itself rather than its true bond strength to the ACKNOWLEDGME NT S
dentin (Bonifácio et al., 2012; Choi et al., 2006). Also, it may be related The authors thank the vice‐chancellery of Shiraz University of
to numerous porosities in the structure of the material, which may act Medical Sciences, for supporting the research (Grant#21193). This
as stress points (Hoshika et al., 2015). In addition, the most adhesive manuscript is extracted from the thesis of Ayda Safarpour. The
failure was found for CAD bonded to Panavia SA. Adhesive failures in authors would like to thank Shiraz University of Medical Sciences,
CAD may be related to several factors like the presence of collagen Shiraz, Iran, also the Center for Development of Clinical Research of
fibrils partially denatured by bacterial acids and/or metalloproteinases Nemazee Hospital, and Dr. Nasrin Shokrpour for editorial assistance.
(Kuboki et al., 1977; Pashley et al., 2004) and an incomplete infiltration
of the luting agent into the demineralized dentin that is commonly CONFLIC T OF INTEREST
related to these failures (Hashimoto et al., 2002). There is no conflict of interest.
Here, we noticed that despite the finding that the Ca/P weight
ratio was higher in the CAD group bonded to both TheraCem and DATA AVAILABILITY STATEMENT
Panavia SA compared to unbonded CAD, there was no significant The data that support the findings of this study are available from the
difference between the two types of cement. It is well known that corresponding author upon reasonable request.
calcium silicate cements, under a wet condition, can release calcium
and form apatite crystals. They can also form calcium hydroxide, which ETHIC S S TATEM ENT
is a highly alkaline material and, hence, may cause degradation of the This study was approved by the Research Ethics Committee of Shiraz
exposed demineralized collagen (Camilleri, 2014; Chen et al., 2018; University of Medical Sciences (Ethical Approval Number: IR.SUMS.-
Huang et al., 2020). Although calcium silicate cements may deliver the DENTAL.REC.1399.191) and conforms with the declaration of
minerals to the demineralized dentin and may increase its hardness, it Helsinki and follows the protection of human subjects' guidelines.
is shown that they cannot induce intrafibrillar remineralization and From all participants, informed written consent was taken.
recovery of a sound modulus of elasticity (Schwendicke et al., 2019).
The observed peaks of ions other than calcium and phosphate may be ORC I D
related to the main component of the cement, also the mineral content Maryam S. Tavangar http://orcid.org/0000-0003-2221-5531
dissolved by the functional acidic monomer, and the filler particles Arefeh Torabi Parizi https://orcid.org/0000-0002-6635-4237
released from the cement itself (AL‐Kataan and Ali 2021).
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