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Year : 2014  |  Volume : 6  |  Issue : 2  |  Page : 86-91

The effect of different irrigating solutions on the push out bond strength of endodontic sealer to dentin and assessing the fracture modes: An In-vitro study

Department of Conservative Dentistry and Endodontics, College of Dental Sciences, Davangere, Karnataka, India

Date of Web Publication28-Oct-2014

Correspondence Address:
Vasundhara Shivanna
Room No.9, Department of Conservative Dentistry and Endodontics, College of Dental Sciences, Davangere - 577 004, Karnataka
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Source of Support: None, Conflict of Interest: None

DOI: 10.4103/2231-0754.143483

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Aim: To evaluate the effect of smear clear, 7% maleic acid, 10% citric acid, and 17% EDTA on the push-out bond strength of epoxy resin-based endodontic sealer to dentin. Materials and Methodos: Fifty extracted mandibular premolars were collected. After decoronation using a diamond disc and water spray to obtain approximately 14 mm long root segments, canal patency and working length were established by inserting K file #15 (Mani). The root canals were enlarged using Protaper nickel-titanium rotary instruments to size #F3 at the working length irrigating with 3 mL of 2.6% sodium hypochlorite between each file size. The roots were then randomly divided into four groups (n = 10) according to the final irrigation regimen Group1: Saline (control). Group 2: 17% EDTA, Group 3: 7% maleic acid, Group 4: 10% citric acid, Group 5: Smear clear. Obturation was done using gutta-percha with AH Plus sealer. Each root section was then subjected to a compressive load via a universal testing machine, to measure the push out bond strength followed by assessment of fracture pattern under stereomicroscope. Results: The data was collected and submitted to statistical analysis by one-way analysis of variance (ANOVA) test. Group 3: NaOCl/maleic acid/distilled water showed greater bond strength (2.2+/-0.278 MPa) as compared to other groups. Mixed type of bond failure was predominant. Conclusion: Removal of smear layer with maleic acid as a final rinse enhanced the adhesive ability of AH plus sealer, followed by EDTA and smear clear.

Keywords: AH plus, bond strength, EDTA, endodontic irrigants, smear layer, smear clear

How to cite this article:
Shivanna V. The effect of different irrigating solutions on the push out bond strength of endodontic sealer to dentin and assessing the fracture modes: An In-vitro study . J Int Clin Dent Res Organ 2014;6:86-91

How to cite this URL:
Shivanna V. The effect of different irrigating solutions on the push out bond strength of endodontic sealer to dentin and assessing the fracture modes: An In-vitro study . J Int Clin Dent Res Organ [serial online] 2014 [cited 2021 Aug 5];6:86-91. Available from: https://www.jicdro.org/text.asp?2014/6/2/86/143483

   Introduction Top

Successful endodontic therapy depends on the three-dimensional filling with an impervious, biocompatible, and dimensionally stable filling material .[1],[2] Since gutta-percha is incapable of adhering to the root canal dentin alone, thus a sealer is required to bond the gutta-percha to dentin and also to obtain a fluid tight seal. [3],[4] Several resin-based sealer materials have been developed in an attempt to minimize the leakage and improve the seal. [3] Epoxy resin-based sealer cements such as AH Plus sealer (Dentsply, Germany) have been widely accepted because of their good physical properties, sealability, adequate biological performance, and microretention to root dentin. [5],[6] Use of irrigants before obturation serves to lubricate the dentinal wall, flush out debris, [7] dissolve organic and inorganic components of the smear layer to clean dentine surface, [8] and improve the bonding ability of resin-based sealers. But studies have shown that these irrigants may alter the chemical composition of the dentin surface, dentin permeability, wettability, or extent of collagen degradation, thus altering the interaction of the dentin with the resin-based sealer. [9] Sodium hypochlorite is the most essential irrigant due to its ability to dissolve pulp tissue and anti-microbial effect but also it decreases the bond strength [10] so in addition, the use of a chelating agent like EDTA is needed for smear layer removal. [11] In endodontics, 7% maleic acid and 10% citric acid has been shown to be effective in removing smear layer due to the low ph. [12] Recently, EDTA-based formulations have been developed as final rinse solutions, such as smear clear (Sybron Endo, Orange, CA) [13],[14] containing EDTA, detergent, and cetrimide. This irrigant was specifically designed for the smear layer removal and root canal cleansing. [15],[16] Despite these studies, little published data was available on its effects on the push-out bond strength of root canal sealer in comparison to other chelating agents.

Therefore, the aim of this study was

  1. To evaluate the effect of EDTA, maleic acid, citric acid, and smear clear irrigating solutions on the push-out bond strength of AH plus sealer.
  2. To assess the failure modes on the debonded surfaces.

   Materials and methodos Top

Fifty freshly extracted mandibular premolars were collected with single roots. Using gracey curettes, the hard deposits were removed and soft deposits were removed by soaking teeth in 5.25 % NaOCl for 20 minutes, followed by rinsing them with saline. Then teeth were stored in 0.1% thymol until further use. Before instrumentation, the teeth were decoronated using a diamond disc and water spray to obtain standardized 14mm long root segments. Working length was established by inserting K file #15 (Mani) 1 mm short of the apex. The root canals were instrumented and enlarged using Protaper nickel-titanium rotary instruments (Dentsply, Germany) to size #F3, 9% taper, at the working length. Irrigation with 3 mL of 2.6% sodium hypochlorite was performed between each file size. The roots were then randomly divided into five groups (n = 10) according to the final irrigation regimen.

GROUP 1: 5 ml of saline 0.9% (control) (NIRLIFE, GUJARAT)

GROUP 2: 5 mL of freshly prepared 17% EDTA (Fischer Scientific, MUMBAI)

GROUP 3: 5 mL of freshly prepared 7% maleic acid (Loba chemicals, MUMBAI)

GROUP 4: 5 mL of freshly prepared 10 % citric acid (Laboratory Rasayan)

GROUP 5: 5 mL smear clear (SYBRON ENDO)

[Figure 1] shows all the materials used in the study. Final rinsing was done for 1 minute in each canal. All canals were then rinsed with copious amounts of distilled water to prevent any carry over effect of the final irrigant being tested. The canals were dried using corresponding protaper paper points (Dentsply, Malleifer). After mixing the AH plus sealer ((Dentsply, Germany), it was applied along the walls of the canals using lentulo spiral. Gutta-percha protaper master cone # F3 (Dentsply Maillefer) was lightly coated with sealer and inserted to the working length. A System B plugger size fine medium (Sybron Endo) was used to condense the master cone to within 5 mm from the working length. Then, backfilling was done using Obtura II thermoplasticized technique at 185 o C (Spartan/Obtura, Fenton, MO) to improve the homogeneity, accuracy, and surface adaptation of Gutta-percha. The roots were placed in 100% humidity for 48 hours to ensure complete setting of the sealer. After setting of the sealer, three horizontal sections of 2-mm thickness each were cut from coronal, middle and apical thirds of each root by using a water-cooled precision saw. Each specimen was marked on its apical surface with an indelible marker, and the exact thickness of each slice was measured using a digital calliper.
Figure 1: Materials used in the study

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Push-out testing

Each root section was then subjected to a compressive load via a universal testing machine (BIET, Davangere, India) whereby the apical surface faced the jig and the jig was contacting only the filling. At a crosshead speed of 1 mm/min using a 1 mm diameter stainless steel cylindrical plunger for coronal section, 0.8 mm for middle sections, and 0.3 mm for apical sections, compressive forces were applied in apico-coronal direction until the gutta-percha was dislodged. The bond strength value in megapascals (MPa) was computed by dividing the maximum load needed to dislodge the filling material in Newtons by the interfacial area (mm 2 ).

Analysis of failure modes

After push-out bond strength evaluation, the failure mode of debonded specimens was analyzed using a stereomicroscope (Olympus SZ61, Olympus Optical Co., Tokyo, Japan). The failure modes were classified according to the following criteria:

  1. Adhesive failure between sealer and dentin;
  2. Cohesive failure within sealer;
  3. Mixed failure.

Statistical analysis

the data were statistically analyzed by using the Statistical Package for the Social Sciences (SPSS) software package (Version 19) with the level of significance set at 0.05, to determine the statistically significant differences between the mean values of the irrigants tested.

   Results Top

When the push−out bond strength values of all three regions (apical, middle, and coronal) were pooled, the mean values for each irrigant group were obtained [Table 1]. Results showed that independent of the root third evaluated, the control (Group1) presented a lower push−out bond strength value (1.3307+/−.022 MPa) than the experimental groups (P < 0.05). Maleic acid (Group 3) as the final irrigant provided the highest mean bond strength values of (2.2+/−0.278MPa) , followed by EDTA (Group 2) with values of (2.19+/−0.107MPa) and smear clear.(Group 5) with a value of (2.15 +/−0.102MPa), but no statistically significant differences between the groups were recorded (P > 0.05). Citric acid group showed bond strength values (1.9+/−0.081MPa) greater than control group but less than Group 5 (2.15+/−0.102MPa).
Table 1: Mean push-out bond strength values (MPa)

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The failure analysis showed that mixed failure mode was predominant among the experimental groups and the adhesive failure mode was predominant in the control group.

[Figure 2] shows the comparison of the values (in MPa) of the groups. [Figure 3] shows the failure mode for saline-ADHESIVE. [Figure 4] shows the failure mode for other groups-MIXED.
Figure 2: Shows the comparison of the push-out bond strength values

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Figure 3: Failure mode for saline-adhesive

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Figure 4: Failure mode for other groups-mixed

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   Discussion Top

The root canal instrumentation produces the smear layer that may also contain bacteria and their by-products, obliterating the dentinal tubules entrance, preventing penetration of the sealers and endodontic materials into the dentinal tubules thereby affecting the adhesion of filling materials to the dentin. [17],[18] The removal of this smear layers facilitates the diffusion of the irrigation solutions, intracanal medication, and increases the apical sealing of the root canal filling. [17],[19] This removal is done with the help of irrigants. Surface treatment of dentin with various irrigants may cause changes in the structural and chemical composition of dentin, thereby changing its solubility and permeability characteristics, therefore affecting the adhesion of materials to the dentinal surface. [20]

AH plus sealer was used for the current study in spite of availability of various newer sealers in the market, it is because AH plus sealer has been shown to have the highest bond strength to root dentin [21] , the reasons quoted for the same are that it is an epoxy resin-based sealer which form covalent bonds with root dentin due to opening of its epoxide ring that has no photo polymerisation system in its composition, thus undergoing homogeneous polymerisation with greater bond strength as compared to other monoblock systems. [22] Also the chemical polymerisation is a slow process which allows for adequate shrinkage stress relaxation in AH Plus sealer.

Final rinse in the present study was done for 1 minute for all the irrigation groups, as it has been seen that use of EDTA longer than 1 minute causes inadvertent erosion [23],[24] and greater demineralising effect on the dentin. [22] Similar effect was noted for maleic acid. [22] Also this time interval most closely relates to the one suited for clinical situation.

Bond strength testing has become a popular method for determining the effectiveness of adhesion between endodontic materials and tooth structure. Various tests used to measure bond strength are micro-tensile strength testing, shear strength testing, and push-out strength testing. The method of testing the bond strength chosen of this study was push out design. Probable reasons are that with this design, it is easy to align samples for testing. It is less sensitive to small variations among specimens and to the variation of stress distribution during load application. [25] Goracci et al. expressed that push-out technique was more reliable and precise than the micro-tensile technique for measurement of bond strength to dentin and should be run to suit the convenience of providing specimens and statistical analysis. Providing 2-mm thick specimens eliminated the probability of non-uniform stress distribution. [26]

The present study also proved that the bond strength of the tested AH plus sealer is differently affected by different final irrigating solutions. In this study, maleic acid (Group 3) showed significantly highest bond strength value (2.2 +/−0.278 MPa) and the saline (Group 1) showed significantly lowest bond strength value. Group 2(17% EDTA) and Group 5 (smear clear) were next to maleic acid but had no significant difference among themselves, though the bond strength values obtained for smear clear were lesser than EDTA. Similar results were obtained by studies done by Ravikumar J et al. who proved that removal of smear layer with maleic acid as a final rinse enhanced the adhesive ability of AH plus sealer, followed by EDTA, citric acid, and MTAD. [36].

Highest bond strength with maleic acid (Group 3) may be because its highly acidic, has a better demineralizing effect specially in apical third of the root canal system, [24] within a shorter period of time, [27] hence completely removes the smear layer, creating efficient micro-retention between the dentinal tubules and the AH plus sealer that might be responsible for greater bonding. [13] This statement is supported by Ballal et al. who conducted a study on decalcifying effect of maleic acid and EDTA and proved that MA decalcifies the root dentin, with most calcium and phosphorus extracted during the first 5 minutes, compared with EDTA. [27] Also, 7% maleic acid produces maximum surface roughness on root canal walls as compared to 17% EDTA [27] that might be responsible for greater micromechanical retention of the sealer with the dentin.

Smear clear which is a combination of 17% EDTA, cetrimide and a detergent was introduced with the motive of obtaining better root canal cleaning and disinfection. It was believed that addition of a detergent (surface active agents) in an irrigating solution would increase the efficiency of the irrigation in smear layer removal and penentration of the sealers into the dentinal tubules thereby enhancing their bonding ability. [28] But our study shows that smear clear could not perform better than EDTA in its effect on improving the bond strength. Similar results were shown by Gopikrishna et al., Kandaswamy et al., Vilanova et al. that the use of EDTA-based protocol groups presented higher push-out bond strength values to AH Plus than saline and the presence of surfactants in smear clear did not increase the bond strength in relation to 17% EDT. [29],[30],[31] Probable reasons may be, firstly, the combination of surfactants does not alter the properties of EDTA-based formulations [32] and smear clear was seen to be as effective as EDTA for residue removal of smear layer from the dentinal root wall. [33],[34],[35] Apparently, the bond strength of smear clear could not be greater than EDTA. Secondly, it could be attributed to the presence of Tween 80 (detergent) that increased wettability and dentin surface energy, therefore increasing intertubular dentin permeability as well as the exposure of collagen matrix and intertubular fluid, which could have negatively affected the adhesion of the hydrophobic AH plus sealer. [36],[37]

Similar effect of the presence of detergent on the decreased bond strength to hydrophobic sealer likes AH plus was seen with MTAD, which is mixture of doxycycline, citric acid and detergent. [36],[37] In these studies, the values of bond strength were significantly lower than EDTA group for the hydrophobic AH plus, unlike the present study with smear-clear. This might be because of the absence of EDTA in MTAD that slightly improved the bond strength. To further support this concept of hydrophobicity or hydrophilicity and its effect on the bond strength, various authors have shown significantly improved bond strength values on final irrigation with MTAD with the bioceramic sealer, [38] due to its hydrophilic nature. On the contrary, such decreased wetting ability of dentin surface treated with 17% EDTA with increased surface tension prohibited the adhesion of materials hydrophilic in nature as ActiV GP, [37] and other methacrylate resin-based sealers like Resilon-Epiphany systems. [39],[40]

Final irrigation with EDTA resulted in higher bond strength values for AH plus than citric acid. This may be attributed to EDTA significantly decreasing the wetting ability of dentinal wall (i.e., decreased surface energy) as compared to citric acid. Attal et al.[39] and Dogen Buzoglut et al.[40] conducted studies on the effect of surface treatment on the free surface energy of dentin using various agents and concluded that the alteration of surface energy gave information on adhesion mechanisms involving hydrophilic and hydrophobic interactions. Therefore, use of agent like EDTA in the present study, that decreases the surface energy could provide a suitable dentin substrate for the adhesion of materials with hydrophobic nature as the resinous AH plus. [39],[40] A study done by Zehnder et al. shows that citric acid has lower surface energy than 17% EDTA, thereby explaining low bond strength on its use as final irrigant with hydrophilic AH plus. [41] Also, the bond strength values recorded for EDTA in the present study are similar to ones reported by Sly et al. [42]

Group 1 saline showed significantly lowest bond strength values. It was because the smear layer was left intact. This was in concurrence to the previous study performed by Eldeniz et al. wherein smear layer removal enhanced the bonding ability of AH plus sealer. [43]

On the assessment of failure pattern under stereomicroscope, it was found that the saline group exhibited adhesive type of bond failure correlating to the results of the study indicating decreased bond strength on irrigation with saline. Other test specimens exhibited predominance of mixed failure (adhesive and cohesive failure). [44]

   Conclusion Top

Within the limitations of this present in-vitro study the following conclusions can be drawn:

  1. Type of dentin pre-treatment has an effect on the adhesive ability of the sealer depending on whether it is hydrophobic or hydrophilic.
  2. Among the irrigants tested, maleic acid provided highest bond strength to AH plus sealer, followed by EDTA and smear clear. Saline had lowest push-out bond strength values among all the groups.
  3. Mixed bond failures dominated among the tested groups.

   Acknowledgment Top

Special thanks to Shipra Gupta, my post graduate student for helping me in making of this paper.

   References Top

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   Authors Top

About the Author Dr. Vasundhara Shivanna received her B.D.S. from Government Dental College, Banglore in 1979 and her M.D.S in branch of conservative & endodontics from Bapuji Dental College 1988. She has an excellent academic career spanning over 32 years. She received fellowship in rotary endodontics in 2007 from International academics of rotary endodontics. She is Dean, Professor and Head of Department of Conservative Dentistry and Endodontics, College of Dental Sciences, Davangere. She is a reviewer for many national and international journals. She also successfully conducted DNB examinations consecutively for 4 years from 2002-5. She has been invited as guest speakers for many national. She has the honor of being the consultant editor for JCD (2003), KSDJ and JICDRO. She was also the member of the editorial board of ENDODONTOLOGY (2003).


  [Figure 1], [Figure 2], [Figure 3], [Figure 4]

  [Table 1]

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