Resistencia en Paredes de Cementos

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Odontology

https://doi.org/10.1007/s10266-020-00535-7

ORIGINAL ARTICLE

Dislodgement resistance and adhesive pattern of different endodontic


sealers to dentine wall after artificial ageing: an in‑vitro study
Galvin Sim Siang Lin1 · Nik Rozainah Nik Abdul Ghani1   · Tahir Yusuf Noorani1 · Noor Huda Ismail2 ·
Noraida Mamat3

Received: 12 May 2020 / Accepted: 26 June 2020


© The Society of The Nippon Dental University 2020

Abstract
To compare the dislodgement resistance and the adhesive pattern of four different endodontic sealers to root dentine walls.
Ninety lower premolars were assigned to five groups (n = 18), Group 1: no sealer (control); Group 2: EndoRez (ERZ); Group
3: Sealapex (SPX); Group 4: EndoSeal MTA (ESA) and Group 5: BioRoot RCS (BRS). They were instrumented up to size
30 taper 0.06 and obturated using single cone technique with matched-taper gutta-percha cones and one of the mentioned
sealers. Six teeth from each group were then randomly subjected to 100, 1000 and 10,000 thermocycles, respectively. 1 mm
slice of mid root region, measuring 6 mm from the apical foramen was prepared and subjected to push-out test under a
Universal Testing Machine. Adhesive patterns of sealers were assessed using a stereomicroscope at 20 × magnification and
classified using a new system. Statistical analyses were performed using two-way ANOVA, complemented by Tukey HSD
and Chi-square tests. ESA and BRS showed significantly higher (p < 0.05) push-out bond strength, followed by SPX, ERZ
and lastly the control, but no significant difference was noted between ESA and BRS (p > 0.05) at 100, 1000 and 10,000
thermocycles, respectively. Both ESA and BRS exhibited a significant higher rate (p < 0.05) of Type 3 and Type 4 adhesive
patterns as the thermocycles increased. ESA and BRS demonstrated higher bond strength and better adhesive pattern to root
dentine wall than SPX and ERZ, especially after artificial ageing.

Keywords  Dislodgement resistance · EndoRez · Mineral trioxide aggregate · Sealapex · Tricalcium silicate

Introduction endodontic sealer due to the fact that gutta-percha itself does
not promote bonding to the dentine wall and eventually this
Successful endodontic treatment includes adequate three- reduces its ability to form a complete seal in the root canal
dimensional sealing of the prepared root canal space to system [2]. In this context, an endodontic sealer is used to
prevent bacterial reinvasion through microleakage [1]. establish a fluid-tight seal at the dentin-sealer and gutta-per-
Gutta-percha is still one of the most used root canal fill- cha core-sealer interfaces [3]. Such adaptation is important
ing materials in endodontic treatment. However, it does not to enhance the bond strength of the materials and prevent
completely fill the root canal system without the use of an dislodgement under high occlusal loads [4].
Several types of endodontic sealer have been introduced
in the past few decades such as resin-based, calcium hydrox-
* Nik Rozainah Nik Abdul Ghani ide-based, glass ionomer cement-based, zinc oxide eugenol-
rozainah@usm.my based, mineral trioxide aggregate (MTA)-based and pure
1
Conservative Dentistry Unit, School of Dental Sciences, tricalcium silicate-based which is also known as bioceramic-
Universiti Sains Malaysia, Health campusKubang Kerian, based sealer [5]. One of the biggest challenges among all
16150 Kota Bharu, Kelantan, Malaysia these sealers is their ability to bond to the dentine wall and
2
Prosthodontics Unit, School of Dental Sciences, to maintain the integrity of the seal in the root canals [3, 4].
Universiti Sains Malaysia, Health campusKubang Kerian, EndoRez (Ultradent Products, Inc., South Jordan, UT), a
16150 Kota Bharu, Kelantan, Malaysia second-generation methacrylate resin-based bondable sealer
3
Paediatric Dentistry Unit, School of Dental Sciences, was introduced to fill the canal using single cone technique
Universiti Sains Malaysia, Health campusKubang Kerian, [6]. It is hydrophilic and exhibits excellent flowability which
16150 Kota Bharu, Kelantan, Malaysia

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Odontology

allows it to flow into accessory canals and dentinal tubules, push-out test and to assess their adhesive pattern using a
thus, promoting resin tag formation for better adhesion to new, simple and systematic classification after artificial age-
the root dentine wall [7]. Calcium hydroxide, a popular and ing. Hence, the first null hypothesis was that there is no
promising component of a root canal sealer is still widely significant difference among all four endodontic sealers in
available in the market owing to its antibacterial properties. terms of the push-out bond strength and adhesive pattern.
Besides, calcium hydroxide-based sealers, such as Sealapex The second null hypothesis was that there is no significant
(Kerr Corporation, Orange, California, USA), also have the difference in terms of the push-out bond strength after 100,
ability to stimulate the healing of periapical tissues [8]. 1000, and 10,000 thermocycles, respectively.
Lately, endodontic sealers based on MTA were intro-
duced. It is a material derived from Portland cement and
was first introduced in the field of dentistry around 1993 [9]. Materials and methods
MTA is also claimed to exhibit excellent physical, mechani-
cal, and biological properties [10]. Recently, EndoSeal MTA Sample size calculation
(Maruchi, Gangwon-do, South Korea), a pozzolan-based
MTA sealer, has been commercialized and is available in Bivariate normal distribution model and correlation
the form of a premixed and preloaded paste stored in an air- (G*Power 3.1.9 for Windows) was used to calculate the sam-
tight syringe, which can be used in various clinical applica- ple size and a minimum sample of 16 teeth for each group
tions, including root canal obturation [4]. A previous study was generated. Another 15% of the samples for each group
also reported that such material demonstrated good sealing were added to account for possible drop-out. Thus, the final
ability in the root canal [11]. In 2016, a new pure tricalcium- sample size was 90 samples.
silicate-based endodontic sealer, BioRoot RCS (Septodont,
Saint-Maur-des-Fossés Cedex, France) was introduced into Preparation of the samples
the market. The powder consists of tricalcium silicate, cal-
cium phosphate, povidone, and zirconium dioxide, whereas This was an in-vitro experimental study involving recently
the liquid part consists of calcium chloride with polycar- extracted lower premolars and ethical approval was obtained
boxylate [3]. Unlike other MTA products, pure tricalcium from the Human Research Ethics Committee USM (Ref.
silicate materials consist of a lesser amount of heavy metals USM/JEPeM/18100482). Ninety mature human lower pre-
such as lead, chromium, and arsenic [12]. This is of prime molars recently extracted due to orthodontic and periodontal
importance in using biomaterials during endodontic treat- purposes with patients’ age ranging from 20 to 40 years old
ment to provide a highly predictable result. were collected. All teeth were inspected to ensure that they
Resistance to the dislodgement of endodontic sealers were free from any restoration, fracture, abrasion, resorption
to root dentine wall is usually evaluated by push-out bond defect, and root caries under a microscope (Leica Microsys-
strength test [3, 4, 6]. It is a mechanical test that uses a tem Imaging Solutions, Cambridge, UK) at a 20 × magnifica-
tensile load which is applied longitudinally to the long axis tion by two blinded examiners. The teeth were then meas-
of the root sample until the core material and sealer are ured using a metal ruler (CLR6, Hu-Friedy Mfg. Co. Inc.,
dislodged or pushed out. The push-out bond strength test Chicago, USA) to include teeth with total tooth length of
is reproducible and fracture occurs parallel to the dentine- 21 mm (± 1 mm) and root length of 12 mm (± 1 mm). The
bonding interface which make it applicable to assess paral- tooth samples were also subjected to radiographic examina-
lel-sided samples even if the bond strength is minimal [13, tion (Planmeca, Helsinki, Finland) to confirm the presence
14]. Another advantage of push-out test is its ability to test of single canal, mature apical foramen, and root canal with
materials within the root canal and it does not require highly Vertucci’s Type 1 classification. All teeth were immersed
sophisticated equipment, which allow push-out test to be in 2.5% sodium hypochlorite (NaOCl) solution (Lenntech,
more favourable than other bond strength tests, such as shear Delfgauw, Netherlands) for 24 h to remove remaining tis-
and tensile tests [15]. Several studies have been conducted to sue debris. Subsequently, access cavities were prepared
determine the dislodgement resistance of various endodontic using a diamond Endo-Access bur, 21 mm, size 4 (Dentsply
sealers using push-out test, but, the published results vary Maillefer, Switzerland) and canal patency was checked using
notably [3, 4, 16, 17]. Furthermore, information regarding size 10 K-file (FlexOFiles; Dentsply Maillefer, Switzerland).
the use of thermocycling process to simulate the physiolog- The working length was established at the apical foramen.
ical ageing of endodontic sealers especially for EndoSeal The canals were instrumented with NiTi rotary files (S5 Sen-
MTA and BioRoot RCS is still sparse in the literature. doline, Tillverkarvägen 6, SE-187 66 TÄBY, Sweden) using
Therefore, the purpose of this in-vitro study was to deter- crown-down technique until size 30, taper 0.06. Copious
mine the dislodgement resistance of different endodontic irrigation using 2.5% NaOCl solution was carried out during
sealers to dentine walls of endodontically treated teeth using instrumentation and 5 ml of 17% ethylenediaminetetraacetic

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Odontology

acid (EDTA) solution (Promega Corporation, Wisconsin, diameter to prevent it from hitting the dentine walls caus-
USA) was used to remove the smear layer. Next, 10 ml of ing an unreliable outcome. The speed was set at 1 mm/min,
normal saline solution (RMBIO, Missoula, Montana) was and the push-out test was performed using a Universal Test-
used as final irrigation to wash out remnants of EDTA in ing Machine (Shimadzu, Japan) until the gutta-percha was
the canals. Paper points size 30 (Dentsply, Maillefer, USA) pushed out. The push-out force was applied from apical to
were used to dry the canals. The samples were then ran- coronal direction due to the tapering shape of the root canals
domly divided into five different groups with 18 samples which might affect the validity of the results if placed from
each. They were categorized as: coronal to apical direction [18]. The maximum force needed
Group 1—gutta-percha (GP) only (control). to cause dislodgement of the core materials was recorded in
Group 2—GP + EndoRez (ERZ). Newton (N).
Group 3—GP + Sealapex (SPX). The push-out bond strength was calculated as follows:
Group 4—GP + EndoSeal MTA (ESA). Push-out strength (MPa) = Maximum loading force (N)/
Group 5—GP + BioRoot RCS (BRS). surface area of dentine walls ­(mm2).
The master GP size 30 tapered 0.06 (Meta Dental Corp, The surface area (­ mm2) was calculated using the conical
Glendale, New York, US) were checked in the canals to frustum surface area formula:
ensure the presence of ‘tug-back’ before obturation and √
the sealers were prepared according to the manufacturer’s 𝜋x r1 + r2 x (r1 − r2 )2 + h2
( )
instructions. Obturation was then carried out using single-
cone technique. The sealer was coated around the canal walls whereby r1 is the radius at the coronal part, r2 is the radius
using matched-taper GP cone before placing the GP into the at the apical part and h is the thickness of the sample which
respective canal. Following obturation, the access cavities is 1 mm.
were acid etched with 37% phosphoric acid (Kerr Corpora-
tion, Orange, CA) for 15 s followed by washing, drying and Adhesive pattern assessment
bonding agent (Kerr Corporation, Orange, CA) application.
Light curing was performed for 15 s and the cavities were The remaining sealer adhering to the dentine walls was
restored with microhybrid resin composite (Zmack Comp, examined and analyzed under a stereomicroscope (Wild
Zhermack, Italy) incrementally with each 2 mm increment M3B; Leica; Heerbrugg, Switzerland) at 20 × magnification
light-cured for 40 s. The final restorations were polished as shown in Fig. 1. The adhesive patterns were recorded
with a composite polishing kit (PN 0310BB, Composite Pol- using a new simple and systematic classification by two
ishing Kit CA, Shofu, CA, USA). All experimental proce- blinded operators. The samples were divided into four
dures were performed by a single expert operator to reduce
the internal bias of the study. The teeth were then placed in
an incubator (Memmert GmbH + Co. KG, Schwabach) at
37 °C, 100% humidity for 72 h to allow complete chemi-
cal setting of the sealers. Six teeth from each group were
randomly selected and subjected to 100, 1000, 10,000 ther-
mocycles, respectively. The samples were placed in a ther-
mocycling machine (TS Series Liquid, Weiss Technik, North
America) with water bath sequence of 5, 37 and 55 °C; dwell
time of 30 s and transfer time of 5 s.

Dislodgment resistance assessment using push‑out


test

After thermal cyclic process, a 1 mm thick horizontal root


slice was cut from the mid-root region of each tooth, meas-
uring 6 mm from the apical foramen using a hard tissue
cutter (EXAKT 312, EXAKT Technologies, Inc., Oklahoma
City, USA). The specimens were microscopically examined
before push-out testing to confirm a circular canal shape and
ensure that the specimens were free from defects such as
Fig. 1  Representative image showing root section viewed under a
void and crack. Samples were then subjected to increasing stereomicroscope at 20 × magnification. (arrow) indicates the sealer
occlusal push-out force with spherical steel tip of 0.6 mm adhered to root dentine wall

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Odontology

quadrants, if sealer was noted in one quadrant, it will be used to analyze the differences in adhesive pattern among
classified as Type 1 adhesive pattern; two quadrants, Type 2 all four endodontic sealers. Significance level was set at
adhesive pattern; three quadrants, Type 3 adhesive pattern p = 0.05.
and if sealer was noted all over the four quadrants, it will
be classified as Type 4 adhesive pattern, which is the most
favourable one. However, if there was no sealer noted on the Results
dentine wall, it will be classified as ‘non-adhesive’.
The results of push-out bond strength are tabulated in
Statistical analysis Table 1 and illustrated in Fig. 2. A significant difference
in bond strength was observed (p < 0.05) with BRS dem-
Data analysis were carried out using SPSS version 24.0 for onstrating the highest mean push-out bond strength fol-
Windows (SPSS Inc., Chicago, IL, USA). Normality test for lowed by ESA, SPX, ERZ, and lastly, the control group at
data distribution was checked with Kolmogorov–Smirnov 100 thermocycles and 1000 thermocycles, respectively.
test. Since data were normally distributed, the dislodgement However, at 10,000 thermocycles, ESA showed the high-
resistance was analyzed using two-way ANOVA comple- est mean value (p < 0.05) followed by BRS, SPX, ERZ
mented by post hoc Tukey HSD test. Chi-square test was and lastly, the control. No significant difference (p > 0.05)

Table 1  Mean push-out bond Number of Type of sealer (SD) p value


strength ­(Nmm−2) of all thermocycles
endodontic sealers tested control ERZ SPX ESA BRS

100 0.648 (0.095) 1.192 (0.073) 1.401 (0.084) 1.846 (0.093)a 1.882 (0.102)a 0.001*
1000 0.568 (0.065)A 1.068 (0.043) 1.201 (0.055) 2.088 (0.069)b 2.123 (0.095)b 0.001*
10,000 0.564 0.912 0.990 2.372 2.338 0.001*
(0.054)A (0.057) (0.064) (0.104)c (0.078)c
*
 Significant at 0.05; SD indicates standard deviation
Same superscript lowercase letters within row indicate no statistical difference (p > 0.05); same superscript
capital letters within column indicate no statistical difference (p > 0.05)

Fig.2  Mean push-out bond strength ­(Nmm−2) of different endodontic sealers

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Odontology

was observed between ESA and BRS at 100, 1000 and Discussion
10,000 thermocycles, respectively. Furthermore, no signif-
icant difference (p > 0.05) was found in the control group The present study evaluated and compared the dislodgement
between 1000 and 10,000 thermocycles. As the number of resistance and the adhesive pattern of four different endo-
thermocycle increased, the bond strength of the ERZ and dontic sealers to root dentine walls after artificial ageing.
SPX decreased significantly (p < 0.05), whereas a statisti- The first null hypothesis was partially rejected, because sig-
cally significant (p < 0.05) increase in the bond strength of nificant differences in terms of the push-out bond strength
ESA and BRS was noted as the thermocycles increased. and adhesive pattern were noted. Although EndoRez can
The adhesive pattern of each endodontic sealer is form a monoblock system in the root canal and create long
demonstrated in Table 2. At 100 thermocycles, most of resin tags that penetrate dentinal tubules to provide a close
the specimens fall in Type 1 adhesive pattern with only adaptation to the dentine walls, low bond strength was still
one specimen in BRS showed Type 3 adhesive pattern reported in the present study which is in accordance with
and no specimen demonstrated Type 4 adhesive pattern. the results found in the literature [16, 17]. The monoblock
Chi-square test did not reveal any significant difference concept aims at achieving a single homogenous unit in the
between the groups at 100 thermocycles (p > 0.05). At root canal system but such entrepreneurial concept has been
1000 thermocycles, the adhesive pattern of ERZ remained hampered by the lack of chemical bond between EndoRez
static, whereas a slight improvement was found in SPX. and gutta-percha [7]. Moreover, intrinsic volumetric shrink-
A significant difference (p < 0.05) was observed among age and the conversion of carbon–carbon double bonds to
the groups in which most of the specimens fell in Type 1 single bond are among the major problems whereby resin
and Type 2 adhesive patterns, whereas only one specimen materials will experience interfacial stress during polymeri-
each in ESA and BRS, exhibited Type 4 adhesive pattern. zation that reduces their bond strength [19]. Also, C-factor is
At 10,000 thermocycles, the adhesive pattern of ERZ and extremely high in the root canal, which will cause debonding
SPX remained unchanged. Majority of the specimens dem- of the material when subjected to huge polymerization stress
onstrated Type 2 adhesive pattern, but most of the speci- [20]. These could be the plausible reasons for inferior bond
mens obturated with ESA and BRS exhibited Type 3 and strength of EndoRez in the present study.
Type 4 adhesive patterns. Overall, these two sealers exhib- Sealapex in the present study showed slightly higher bond
ited significantly better adhesive property (p < 0.05) than strength than resin sealer probably due to the interaction
ERZ and SPX as the number of thermocycles increased. between isobutyl salicylate which is found in the material
itself and also calcium in the tooth that formed a chemical

Table 2  Adhesive pattern of all Type of sealer Type of adhesive pattern, η p value


endodontic sealers tested
non-adhesive Adhesive
1 2 3 4

100 Thermocycles
 ERZ 3 3 0.131
 SPX 3 2 1
 ESA 3 3
 BRS 2 3 1
1000 Thermocycles
 ERZ 3 3 0.049*
 SPX 2 2 2
 ESA 2 2 1 1
 BRS 3 2 1
10,000 Thermocycles
 ERZ 3 3 0.028*
 SPX 2 2 2
 ESA 2 3 1
 BRS 2 2 2
*
 Significant at 0.05

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Odontology

barrier [21]. Despite this, calcium hydroxide sealer will 14]. Moreover, it is also challenging to assess the cohesive-
degrade and dissolve over time [22]. This elucidates the ness of an endodontic sealer in push-out test as the loading
decreased bond strength of Sealapex as the thermocycles jig-covered part of the sealer in which internal validity is
increased. Bioceramic sealers, (EndoSeal MTA and BioRoot questionable. Currently, very limited studies focus on the
RCS) on the other hand, showed higher bond strength than adhesive pattern of these sealers to dentine walls. A new sys-
other sealers due to the formation of apatite layer, intrafi- tematic classification is introduced in this study to identify
brillar apatite deposition and also tag-like structures that the type of adhesive pattern of sealer to root canal dentinal
form mineral plugs along with the dentine bonding interface, wall, which provides a more applicable and simple method
known as the mineral infiltration zone [4, 12, 23]. Addi- to assess the adhesiveness of the materials. To the best of
tionally, bioceramic sealers undergo bioactivity process that our knowledge, there is yet no standardization in assessing
results in apatite nucleation, which prevents dislodgement the adhesive pattern of endodontic sealers, because no con-
of the gutta-percha from the canal and provides a tight seal sensus on evaluation parameters has been reached among
in the root canal system [24]. Howbeit, a direct comparison researchers. It is important to emphasize that the adhesive
with other push-out bond strength studies is not pertinent as property of sealers is somewhat correlated to the bond
the compared materials are greatly different and huge design strength which is shown in the results of the present study.
variability occurred in the methodology among studies. Thermocycling process has been introduced as one of
It has been claimed that push-out bond strength test is not the most widely used and valid in-vitro tests to simulate and
advisable for gutta-percha as it will undergo plastic deforma- accelerate the physiological ageing of material in a clinical
tion during testing [15]. Suggested solutions to this problem setting [25]. The thermal test will stress the bond between
included the filling of canals entirely with sealer without any the materials and the dentinal walls which will further impair
core material [6]. However, the interest of simulating clinical the bond strength of the materials itself [26]. However, the
conditions in a natural root canal is lost. Since the present use of thermocycling for endodontic sealers remains con-
study aimed to compare the dislodgement resistance of vari- troversial, as several authors questioned the use of thermal
ous endodontic sealers in a clinically orientated setup, thus, test on materials in the root canals. Studies have shown that
the sealers were used with gutta-percha cone that is recom- cement material will be affected by thermal changes due
mended by the manufacturer. Notwithstanding, the push-out to difference in coefficient of thermal expansion, and lead
test is still a significant tool to rank the bonding ability of to a decrease in bond strength causing microleakage and
different endodontic sealers and the rankings are reported to bonding failure [27, 28]. Even though the root is embedded
be similar when comparing canals filled with gutta-percha in the bone, but due to the thermophysical properties of a
with those filled with sealer alone [6]. Other variables such tooth [29], the temperature experienced by the crown will be
as the punch diameter, root canal preparation, obturation transferred to the root as well [30]. This provides concrete
technique, specimen thickness and specimen orientation evidence that thermal test is a reliable method to simulate
should be addressed systematically to avoid internal bias ageing of root canal materials.
[15]. In the present study, the punch diameter used was set The second null hypothesis was partially rejected since
at 0.6 mm which is within the acceptable range as a punch all sealers demonstrated significant changes as the thermo-
diameter between 70 and 90% of the canal diameter will not cycles increased except for the control group. EndoRez and
cause significant effect on the results [15]. Besides, a taper Sealapex showed decreased bond strength with increased
of 0.06 was used in the present study, because such taper will thermocycles, but EndoSeal MTA and BioRoot RCS showed
create an angulation of only 3.5° to allow very small effect a contrasting result which is inconsistent with a previous
on the frictional resistance during the push-out test [15]. In study [28]. From a clinical standpoint, the biomineraliza-
addition, single cone technique was used as lateral conden- tion process of bioceramic sealers enhances the dislodge-
sation and warm vertical techniques were found to cause a ment resistance to root dentine walls by forming a colloi-
negative impact on the push-out force [3]. Thus, these test- dal calcium silicate hydrate gel that will harden and create
ing protocols should be performed appropriately to provide a micromechanical interaction by tag-like structures over
better standardization of the push-out test. time [3, 12]. Therefore, one may hypothesize that the bond
The current study highlights the importance of adhesive strength of bioceramic sealers will not deteriorate even after
properties of endodontic sealers to improve the bonding abil- being subjected to a series of thermocycling processes due
ity, and to maintain the integrity of the seal in the root canal to the continuous hardening and improved adhesion from the
in both static and dynamic states [14]. Previous studies clas- hydration reaction which make them difficult to dislodge.
sified the failure mode of endodontic sealers into adhesive, Such observation also corroborates another clinical finding,
cohesive or combination of both adhesive and cohesive pat- that the retreatment of bioceramic sealing material is more
terns, but none of them could correlate these failure modes difficult and requires more time to be removed since the
with the bond strength of various endodontic sealers [3, 4, 6, sealer remnants adhered strongly to the root dentine walls

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Odontology

even after a period of 2 weeks [31]. Nonetheless, the expla- References


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