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This article has been accepted for publication and undergone full peer review but has not

been through the copyediting, typesetting, pagination and proofreading process which may

lead to differences between this version and the Version of Record. Please cite this article as

an 'Accepted Article', doi: 10.1111/iej.12257

This article is protected by copyright. All rights reserved.

Received Date : 12-Aug-2013

Accepted Date : 27-Jan-2014

Article type : Original Scientific Article

The bond strength of endodontic sealers to root dentine exposed to different gutta-percha

solvents

H.S. Topuolu 1, S. Demirbuga 2, . Tuncay 1,H. Arslan 3,B. Kesim1, B. Yaa4

1Department of Endodontics, Faculty of Dentistry, Erciyes University, Kayseri, 2Department of

Restorative Dentistry, Faculty of Dentistry, Erciyes University, Kayseri, 3Department of Endodontics,

Faculty of Dentistry, Katip elebi University, Izmir, 4Department of Restorative Dentistry, Faculty of

Dentistry, Katip elebi University, Izmir, Turkey

Running Title:Bond strength of endodontic sealers

Key words: Bond strength, Root dentine, Sealer, Solvent

Address for correspondence/reprints:

Dr. Hseyin Sinan TOPUOLU

Department of Endodontics, Faculty of Dentistry, Erciyes University,

Melikgazi, Kayseri, TURKEY Zip code: 38039

Tel: +90 (352) 207 66 66


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Fax: +90 (352) 438 06 57

E-mail: [email protected]

Abstract

Aim To evaluate the effects of various gutta-percha solvents on the push-out bond strength of several

root canal sealers on root dentine.

Methodology The root canal of two hundred and ten single-rooted human teeth were prepared with

the ProTaper System (Dentsply Maillefer, Ballaigues, Switzerland) up to a master apical file size of

F4 and the following variables evaluated for bond strength: solvent type (chloroform, eucalyptol, and

orange oil), time (2 and 5 minutes), sealer type (AH Plus, MTA Fillapex, and Sealapex), and root

thirds (coronal, middle, and apical). After canal filling, three 1-mm-thick slices were obtained from

each root sample and the bond strength of the test materials were measured using a push-out test setup

at a cross-head speed of 1mm/min. The data were analyzed using four-way factorial ANOVA (P =

0.05).

Results Bond strength was significantly affected by solvent type and time (P < 0.001). The use of

chloroform for 5 minutes in the root canal decreased bond strength of all sealers (P < 0.001).

Eucalyptol and orange oil did not affect the bond strength of the sealers (P > 0.05). In all conditions,

the push-out bond strength was highest for AH Plus and lowest for MTA Fillapex (P < 0.001). Bond

strength values decreased in a corono-apical direction in all groups (P < 0.001).

Conclusions Chloroform used for 5 minutes during retreatment decreased the bond strength of AH

Plus, Sealapex, and MTA Fillapex to root dentine.

Introduction

The success of root canal treatment depends on completely cleaning and shaping, and then filling the

root canal systems. If these parameters are not achieved, post-treatment disease may occur because of

the persistence of bacteria in the root canal system (Siqueira 2001). When this occurs, non-surgical

root canal retreatment is often indicated as the first choice to eliminate the microbial infection. The


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retreatment aims to completely remove the old filling material from the root canal system to allow

effective cleaning, shaping, and refilling of the root canal (Kvist & Reit 1999, Mollo et al. 2012).

In root canal retreatment, solvents are often used as an aid for removing gutta-percha.

Chloroform, an organic solvent, has been shown to be effective when used with gutta-percha (Wilcox

1995, Schafer & Zandbiglari 2002), however, it has carcinogenic potential (Vajrabhaya et al. 2004)

and the search for alternative solvents continues (Hunter et al. 1991). Studies have shown that

essential oils, such as eucalyptol, orange oil, and turpentine oil, may be used in retreatment because

they are safe and useful for dissolution of gutta-percha and root canal sealers (Uemura et al. 1997,

Hansen 1998).

Several chemical agents change the chemical structure of dentine and the Ca/P ratio of dentine

surfaces. Alterations in the original Ca/P ratio between organic and inorganic components may

change the permeability and solubility of root dentine and can affect the adhesion of dental materials

to hard tissues (Hennequin et al. 1994, Rotstein et al. 1996). During root canal retreatment, the root

and coronal dentine is exposed to gutta-percha solvents deposited in root canals. Kaufman et al.

(1997) reported that solvents may alter the chemical composition of dentine surface and affect bond

strength of restorative materials to dentine.

Many studies have been conducted to evaluate the effects of various endodontic procedures on

the bond strength of root canal sealers (Amin et al. 2012, Haragushiku et al. 2010, Vilanova et al.

2012). However, there is no information about the effects of various gutta-percha solvents used over

different application times on the bond strength of sealers to root dentine. The purpose of this study

was to compare the push-out bond strength of different endodontic sealers to root dentine exposed to

various gutta-percha solvents for 2 or 5 minutes. The null hypothesis is that various gutta-percha

solvents do not affect the bond strength of several root canal sealers.

Materials and Methods

Two hundred and ten freshly-extracted, straight, single-rooted human mandibular premolar

teeth were selected and stored in distilled water until required. Preoperative mesiodistal and

buccolingual radiographs were taken to verify the presence of a single canal. Criteria for tooth


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selection included a completely formed apex and absence of previous root filling, resorption, or

calcifications. To ensure standardization, crowns of the selected teeth were partially removed to

achieve a final length of 21 mm for each tooth. The crowns served as a reservoir for the solvent.

Endodontic access cavities were prepared using diamond burs (Diatech, Coltene Whaledent,

Altststten, Switzerland)with a high-speed hand piece under water cooling. A size 10 K-file (Dentsply

Maillefer, Ballaigues, Switzerland) was then placed in the canal until it was visible at the apical

foramen. The working length was determined by substracting 1 mm from this measurement. The 210

roots were instrumented with the ProTaper rotary system (Dentsply Maillefer) up to size F4 (size 40,

0.06 taper) as the master apical file. During preparation, the root canal was irrigated with 5 mL of

2.5% sodium hypochlorite (NaOCl) solution using a syringe and a 30-gauge needle (NaviTip;

Ultradent, South Jordan, UT, USA) between each instrument change.

A total of 210 roots were then randomly assigned to 6 experimental groups (n = 30) according

to the solvent type and time of exposure and 1 control group (n = 30) as follows:

Group 1:was not exposed to any solvent (Control); Group 2:Chloroform for 2 min; Group 3:

Chloroform for 5 min; Group 4: Eucalyptol for 2 min; Group 5: Eucalyptol for 5 min; Group 6:

Orange oil for 2 min; Group 7:Orange oil for 5 min.

A total of 0.2 mL of each solvent was placed in the root canal, and left in place up to

completion of the exposure time, and then removed with paper points (Dentsply Maillefer). All canals

received a final rinse of 5 mL 17% EDTA for 1 minute followed by 5 mL distilled water and dried

with absorbent paper points. The roots within each of the six experimental groups and the control

group were further randomly assigned to three subgroups (n = 10) according to the sealer used as

follows: AH Plus(Dentsply DeTrey GmbH, Konstanz, Germany), MTA Fillapex (Angelus, Londrina,

PR, Brazil), and Sealapex (Kerr, Romulus, MI, USA). Each sealer was mixed according to

manufacturers instructions for use. All canals were filled using the single-cone technique with F4

gutta-percha cones (Dentsply Maillefer) .

Following canal filling, mesio-distal and bucco-lingual radiographs were taken to confirm

complete filling. The coronal 1 mm of filling material was then removed and the spaces were filled


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with a temporary filling material (Cavit, 3M ESPE, Seefeld, Germany). After being wrapped in pieces

of sponge, all the specimens were stored at 37C in 100% humidity for 2 weeks.

Push-out testing

The specimens were sectioned horizontally into three 1 0.1 mm thickness serial slices by

using a low-speed precision diamond saw (Isomet; Buehler, Lake Bluff, IL, USA) under continuous

water irrigation. The thickness of each slice was measured with a digital caliper (Teknikel, Istanbul,

Turkey) with an accuracy of 0.001 mm. Both apical and coronal aspects of the specimens were then

examined microscopically to confirm a circular canal shape. The push out test was performed in a

universal testing machine (Instron 4444; Instron Corp., Canton, MA, USA) by applying a continuous

load to the apical side of each slice using 0.7, 0.8, and 0.9 mm diameter cylindrical plungers,

matching the canal diameter of each third. The diameter of each plunger was approximately 90% of

the canal diameter. Loading was applied at a crosshead speed of 1 mm/min from the apical to the

coronal direction until bond fracture occurred. The maximum load applied to filling material before

fracture was recorded in newtons and converted to megapascals (MPa) according to the following

formula (Nagas et al. 2007):

Push-out bond strength (MPa) = N/A

where N = maximum load (N), A = adhesion area of root canal filling (mm

2

).

The adhesion surface area of each section was calculated as: (r1+ r2) xL, where L = (r1

r2)2 + h2; where = 3.14, r1and r2= smaller and larger radii respectively and h= thickness of the

slice in mm.

Analysis of failure modes

After measurement of bond strength, both sides of the failed bond were examined under a

stereomicroscope (BX60; Olympus, Tokyo, Japan) at 30x

magnification to determine the mode of

fracture. The fracture mode was classified according to the following criteria: adhesive fracture at the

sealer-dentine or sealer-core material interface, cohesive fracture within sealer, and mixed fracture in

both the sealer and dentine (Skidmore et al. 2006). Two specimens that were representative of the


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fracture modes from each group were further evaluated under a scanning electron microscope (SEM)

(Leo-440; LEO Electron Microcopy, Ltd., Cambridge, UK).

Statistical analysis was carried out using four-way factorial ANOVA (P = 0.05) at the 95%

confidence level. All statistical analyses were performed using SPSS 16.0 software (SPSS Inc.,

Chicago, IL, USA).

Results

The mean and standard deviations of the groups are summarized in Table 1. All variables had

a significant effect on the push-out bond strength of sealers (P < 0.001) (Table 2). There was a

significant effect regarding the sealer type-root thirds (P = 0.005). The most significant interaction

was between solvent and time followed by time and root third (Table 3).

The use of chloroform for 5 min significantly reduced the push-out bond strengths of all

sealers when compared with other groups (P< 0.001) (Table 1). There were no statistically significant

differences between the control, orange oil, and eucalyptol groups.

Under all conditions, a statistical ranking for bond strength values was obtained as follows (P

< 0.001): AH Plus > Sealapex > MTA Fillapex. The bond strength values were highest in the coronal

and lowest in the apical thirds (P< 0.001).

The modes of fracture are listed in Table 4. Adhesive fracture at the sealer-dentine interface

was the most frequent type of fracture in experimental groups and cohesive fracture was the most

frequent in control group.

Discussion

Adhesion, one of the required physical properties of filling materials, is a desirable property

in root canal sealers (Grossman 1976). Adhesion of an endodontic sealer is defined as its capacity to

adhere to the root canal walls and the ability to promote the union of the core filling materials to each

other and to the dentine (Sousa-Neto et al. 2005, Rached-Junior et al. 2009). In static circumstances,

the adhesion provided by canal sealers eliminates space that might otherwise allow fluid to infiltrate

the sealer-dentine interface (rstavik et al. 1983). In dynamic situations, the adhesion of root canal


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sealers to radicular dentine is beneficial for preserving the integrity of the sealer-dentine interface

during tooth flexure, operative procedures, or the preparation of post space (Saleh et al. 2003,

Huffman et al. 2009).

In retreatment, the solvent is expected to dissolve as much gutta-percha as possible (Faria-

Junior et al. 2011). Several laboratory studies have been carried out to determine the most effective

solvent and application time for dissolving gutta-percha and sealers (Martos et al. 2011, Schafer &

Zandbiglari 2002, Magalhaes et al. 2007, Bodrumlu et al. 2008). Most of these studies have been

evaluated for the effectiveness of different solvents for application times of 1, 2, 5, or 10 minutes and

the results showed that dissolution may vary depending on the solvent type and time of exposure.

During the retreatment process, it is inevitable that solvents will be in contact with the root canal

walls for a period of time. Based on this information, the bond strength of various sealers to root

dentine exposed to different solvents for two different time periods was tested.

Shokouhinejad et al. (2010) evaluated push-out bond strength of Resilon/Epiphany Self-etch

to root dentine after retreatment. They filled the canals and then removed the initial root filling with a

combination of retreatment files and solvent. After retreatment, the roots were refilled with

Resilon/Epiphany Self-etch. In the present study, however, in order to limit the number of variables,

an initial root canal filling was not attempted. Residual filling material that was not equal in all

specimens may remain in the root canal after retreatment procedures (Rdig et al. 2013) and this may

affect the push-out bond strength of material tested in retreatment (Rached-Junior et al. 2013). The

present study, therefore, was undertaken to investigate the direct effects of the solvents to bond

strength of sealers to dentine.

The results of the present study revealed that most interaction was between solvent type and

time. The use of chloroform for 5 minutes had a negative effect on the bond strength of all sealers.

Similarly, a previous study reported that chloroform used for retreatment had an adverse effect on the

bond strength of Resilon/Epiphany SE after refilling of root canal (Shokouhinejad et al. 2010). It has

also been reported that chloroform and halothene decreased bond strength of C&B Metabond (Parkell

Inc., Farmingdale, NY, USA) to root canal dentine (Erdemir et al. 2004). Erdemir et al. (2004)

reported that chloroform and halothene had an effect on the mineral content of root dentine. In the


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current study, the decreased bond strength in the roots exposed to chloroform for 5 min may be

explained by compositional changes in dentine that may affect the bond strength of filling materials.

However, the use of orange oil and eucalyptol for 2 and 5 minutes did not affect bond strength of the

root sealers. Therefore, within the limitations of the present study, the null hypothesis was rejected.

In the present study, AH Plus had the highest push-out bond strength under all conditions.

This result is similar to those in previous studies (Amin et al. 2012, Ersahan & Aydin 2010, Nagas et

al. 2012) that reported the superiority of epoxy resin-based sealers compared to the other sealers used

in this study (MTA Fillapex, Sealapex). The superior results of AH Plus may be due to better

adhesion to root dentine and deeper penetration into dentinal tubules (Lee et al. 2002, Mamootil &

Messer 2007). In the present study, MTA Fillapex had the lowest bond strength values. Sagsen et al.

(2011) claimed that MTA Fillapex exhibited low bond strength because of its low adhesion capability.

Based on these results, it can be concluded that there is an interaction between low adhesion capacity

and low push-out bond strength of MTA Fillapex. Interestingly, and different from previous studies

(Picoli et al. 2003, Lee et al. 2002) considerably higher bond strength values for Sealapex were found

in the present study. These differences may have been a result of the different test methodologies used

to determine the bond strength.

In the present study, single F4 gutta-percha points matched to the final rotary file were used.

It has been suggested that these tapered gutta-percha cones matched to the size and taper of the master

apical rotary files could fill the root canal effectively when used as a single cone (Gordon et al.2005).

A single-cone filling may be regarded as advantageous, because the ultimate filling is composed

mostly of a homogeneous mass of gutta-percha instead of sealer and voids that may be entrapped

among the distinct gutta-percha points when using lateral compaction. Nagas et al.(2009) compared

the bond strength of master gutta-percha points with different tapers (0.02, 0.04, and 0.06) in canals

instrumented with a 0.06 tapered master apical file and found that the 0.06 tapered single-cone

matched to the master apical rotary file provided the highest bond strength.

In the current study, three plunger sizes were used to match the diameter of each of the root

thirds. This avoids excessive pressure on the surrounding root canal walls and any notching effect of

the plunger into the gutta-percha surface. According to the root thirds, bond strength values in all


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specimens were: coronal > middle > apical. This finding is similar to the results of a previous study

(Neelakantan et al. 2012). The penetration of endodontic sealers into dentinal tubules achieves

mechanical locking and may increase retention of the root filling (Mamootil & Messer 2007). The

decreasing bond strength in the corono-apical direction can be explained by the decreasing tubule

density in a coronal to apical direction, which reduces sealer penetration into the smaller tubules in the

apical third (Carrigan et al. 1984, Paque et al. 2006). In the present study, inspection of the root slices

revealed that the fracture modes were mainly adhesive (sealer-dentine interface) for all other groups

except the control group (Table 4). This result may be attributed to changes likely in the chemical

structure of the root dentine exposed to solvents.

Conclusions

The bond strength of AH Plus, MTA Fillapex, and Sealapex were negatively affected by the

use of chloroform for 5 minutes. Further study should evaluate the effect of different solvents for

various periods of time on the bond strength of different sealers.

Acknowledgments

The authors wish to thank Assist. Prof. Blent zkan, Department of Biostatistics and

Medical Informatics, Faculty of Medicine, Izmir Katip Celebi University, for his assistance in

statistical analysis. The authors deny any conflicts of interest related to this study.

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Table 1.Mean standard deviations of push-out bond strength values (MPa) for each sealer, solvent, third and time period

Control Chloroform Eucalyptol

Coronal Middle Apical

Coronal Middle Apical Coronal Middle Apical

2min

5min

2min

5min

2min

5min

2min

5min

2min

5min

2min

5min

2m

AH Plus7.20

0.845.57

0.474.24

0.356.30

0.374.72

0.475.38

0.513.43

0.614.43

0.403.01

0.537.44

0.576.34

0.525.87

0.585.350.41

4.280.58

4.340.46

6.0

MTA

Fillapex

2.370.41

1.19

0.28

1.01

0.08

2.27

0.27

1.24

0.34

1.45

0.33

0.81

0.22

1.03

0.38

0.64

0.47

2.38

0.40

2.11

0.33

1.37

0.46

1.52

0.77

0.89

0.31

0.71

0.20

2.

0

Sealapex3.30

0.70

2.67

0.47

1.42

0.40

3.23

0.28

1.65

0.40

2.31

0.32

1.40

0.46

1.58

0.38

0.94

0.19

3.13

0.23

2.83

0.46

2.39

0.37

2.44

0.31

1.44

0.36

1.50

0.37

3.

0

cce

pted

Ar

ticl


15/15

Acc

eptedA

rticle


Table 2. Summary of the statistical analysis showing the main effects of solvent, time, sealer, and

third on bond strength

Variable F value P value

Solvent 104.719 < 0.001

Time 186.188 < 0.001

Sealer 4071.08 < 0.001

Third 762.15 < 0.001

Table 3.Summary of interactions between variables

Interaction F value P value

Solvent-Time 66.189 < 0.001

Solvent-Sealer 13.904 < 0.001Solvent-Third 7.914 < 0.001

Time-Sealer 3.652 0.027

Time-Third 27.124 < 0.001

Sealer-Third 3.81 0.005

Solvent-Time-Sealer 8.059 < 0.001

Solvent-Time-Third 1.972 0.048Time-Sealer-Third 1.933 0.103

Solvent-Time-Sealer-Third 1.731 0.088

Table 4. Distribution of failure modes

AHPlus+GP MTA Fillapex+GP Sealapex+GP

A1 A2 C M A1 A2 C M A1 A2 C M

Control (n=90) 7 4 15 4 8 3 17 2 5 4 18 3

Chloroform for 2 min (n=90) 13 8 8 1 12 7 9 2 10 9 8 3Chloroform for 5 min (n=90) 14 6 9 1 10 9 8 3 13 10 7 0

Eucalyptol for 2 min (n=90) 16 7 6 1 12 10 6 2 9 14 6 1

Eucalyptol for 5 min (n=90) 8 13 9 0 17 8 5 0 14 11 5 0

Orange oil for 2 min (n=90) 15 7 6 2 14 9 6 1 21 9 0 0

Orange oil for 5 min (n=90) 16 4 7 3 20 1 9 0 18 6 5 1

A=adhesive (A1=sealer/dentine interface, A2=sealer/core material interface); C=cohesive; M=mixed. GP=gutta percha.

Ret Solventes Cimentos

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