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Basic Research—Technology

Interfacial Adaptation of Adhesive Materials to Root Canal Dentin

Jorge Perdigão, DMD, MS, PhD,* Maria M. Lopes, BS, and George Gomes, DMD

Abstract

Extracted single-rooted maxillary teeth were endodon- tically treated and filled with gutta-percha/AH-26 (GP), Resilon points/RealSeal (RS), AdheSE DC/Multicore Flow (ADH, self-etch control), or Excite DSC/Multicore Flow (EXC, total-etch control). Specimens were ana- lyzed with electron microscopy using three methods: (a) field emission scanning electron microscopy (FESEM) of the interface; (b) transmission electron microscopy (TEM) of the interface; and (c) FESEM of the material fitting surface. The three adhesive materials (RS, ADH, and EXC) formed a dentin hybrid layer, which nonethe- less resulted in interfacial separation. Gaps were more frequent for GP, which did not hybridize dentin. The fitting surfaces exhibited resin tags at all levels for EXC. Tags were less frequent with ADH, especially in the apical third. For RS, resin tags were rare and virtually absent from the apical half, whereas GP did not form tags. Despite the hybridization, a tight seal of the root canal is difficult to achieve because of the complexity and the mechanical challenge of the substrate. (J Endod 2007;33:259 –263)

Key Words

Dental bonding, electron microscopy, Resilon, resin cements, root canal obturation

From the *Division of Operative Dentistry, Department of Restorative Sciences, University of Minnesota, Minneapolis, Minnesota; School of Medicine and Dentistry, University of Santiago de Compostela, Santiago de Compostela, Spain; and the School of Dentistry, University of Granada, Granada, Spain. Address requests for reprints to Dr. Jorge Perdigão, Uni- versity of Minnesota, Division of Operative Dentistry, Depart- ment of Restorative Sciences, 8-450 Moos Tower, 515 SE. Delaware St., Minneapolis, MN 55455. E-mail address:

perdi001@umn.edu.

0099-2399/$0 - see front matter Copyright © 2007 by the American Association of Endodontists.

doi:10.1016/j.joen.2006.10.002

JOE — Volume 33, Number 3, March 2007

T he goal of root canal therapy is to eliminate intracanal bacteria and to seal the root canal system and crown access with materials that prevent reinfection ( 1, 2 ). Gutta- percha is considered the gold standard root canal filling material ( 3 ). Adhesives have been used primarily to bond restorative materials to coronal enamel and dentin ( 4, 5 ). More recently, adhesives have been used in the root canal to bond posts and to strengthen endodontically treated teeth ( 6 –11 ). However, most attempts to seal the root canal system with adhesives have proved unsuccess- ful ( 11–15 ). A new root canal filling material has been recently developed ( 16 ). This material

is composed of a thermoplastic polycaprolactone-based filled polymer (Resilon, Resi-

lon Research LLC, Madison, CT) combined with proprietary self-etching adhesive and a dual-cured composite resin sealer ( 17 ). Controversy has recently emerged concerning the use of this material. According to one research group, the Resilon system forms a monoblock between the root canal dentin and the respective filling material ( 9, 18 ), resulting in a lower incidence of apical leakage but strengthening the tooth ( 9, 18 ). However, the findings of a different research group challenged both the sealing ability of the monoblock concept ( 17 ) and its potential for reinforcing the residual tooth structure ( 19). Self-etching and total-etching dual-cured adhesive systems have been extensively tested; therefore, they serve as appropriate controls to test the new polycaprolactone- based filled polymer. The purpose of this study is to compare the interfacial ultramor- phology and sealing ability of RealSeal sealer/Resilon points with that obtained with gutta-percha/AH-26 sealer, using two resin adhesive systems as controls. The null hypothesis tested is that the dentin penetration and sealing ability of the new root canal filling material is not superior to that of existing materials.

Materials and Methods

We used 36 single-rooted human maxillary teeth stored in 0.2% chloramine at

4°C. Access was made with a tapered round end bur (Brasseler USA, Savannah, GA) with

a high-speed handpiece and water spray. For working length calculation, 1 mm was

subtracted from the total length of the file inside the root canal. A crown-down tech- nique was used for instrumentation with Gates Glidden (Moyco Union Broach, York, PA) #2 to #4 drills and then rotary files (Profile .06 Taper Series 29, Dentsply Maillefer, Tulsa, OK) were used incrementally up to a #35 file/.06 taper. The teeth were irrigated between each instrument, and the canal space was filled with irrigant during the instru- mentation phase. For each tooth, 2 ml of 5.25% sodium hypochlorite (NaOCl) (The Clorox Co, Oakland, CA) was delivered with a Monoject syringe (Sherwood Medical Co., St. Louis, MO) and a 27-gauge needle. The final rinse was done with 5.25% NaOCl followed by 2 ml of distilled water. The canal spaces were dried with absorbent paper points (Dentsply Maillefer, Tulsa, OK) and randomly divided into four groups.

Group 1: Gutta-Percha and AH-26 (GP)

The canals were coated with AH-26 (Dentsply Maillefer) using paper points dipped into the sealer. The warm vertical condensation technique was accomplished with Obtura II (Obtura Spartan, Fenton, MO) warm gutta-percha and Obtura warm gutta-percha condensers (S-Kondensers, Obtura Spartan).

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Group 2: RealSeal (RS)

RealSeal Primer (Sybron Endo, Glendora, CA) was introduced into the root canal with a disposable brush, and excess primer was removed with paper points. A nonstandardized RealSeal master cone (made of Resilon, Resilon Research LLC) was tried-in to within 1 mm of working length. RealSeal root canal sealant was then placed into the root canal using a paper point. After placing the master cone to the working length, the lateral condensation technique was accomplished with a stainless steel finger spreader (Moyco Union Broach) and medium-fine acces- sory cones dipped in resin sealer. The excess material was seared off and condensed with a plugger 1 mm below the canal opening. The material was then light cured for 40 seconds with a XL2500 curing unit (3M ESPE, St. Paul, MN).

Group 3: Excite DSC and Multicore Flow (EXC)

The canals were etched with 37% phosphoric acid gel (Total Etch, Ivoclar Vivadent, Schaan, Liechtenstein) for 15 seconds, rinsed, and excess water was absorbed with paper points. The dual-cured adhesive Excite DSC small/endodontic size (Ivoclar Vivadent, Schaan, Liechten- stein) was applied, and excess bonding agent was removed with paper points. Multicore Flow (Ivoclar Vivadent, Schaan, Liechtenstein) was injected into the canal with a unit-dose needle tip (Bisco Inc., Schaum- burg, IL) starting at the apical end of the canal. The light guide was placed at the access opening and activated for 60 seconds.

Group 4: AdheSE DC and Multicore Flow (ADH)

AdheSE primer (Ivoclar Vivadent, Schaan, Liechtenstein) was ap- plied into the root canal with a disposable brush, and excess primer was removed with paper points. AdheSE Bonding and AdheSE DC Activator were mixed and applied into the root canal with a disposable brush. Excess bonding was removed with paper points. Multicore Flow (Ivo- clar Vivadent, Schaan, Liechtenstein) was injected into the canals and light cured as for group 3. The openings were sealed with Cavit (3M ESPE). Teeth were stored in 100% humidity in black film containers for 7 days. Three teeth of each group were randomly assigned to one of three methods.

Analysis of the Interface Using a Field-Emission Scanning Electron Microscope (FESEM) Teeth were sectioned perpendicularly to the long axis with a dia- mond saw (Isomet 1000, Buehler Ltd., Lake Bluff, IL) under distilled water to obtain 1.5 0.2-mm-thick slices. The specimens were im- mersed in 2.5% glutaraldehyde/2% paraformaldehyde in 0.1 M sodium cacodylate buffer at pH 7.4 for 12 hours at 4°C and thoroughly pro- cessed to hexamethyldisilazane ( 20 ) drying (HMDS, Ted Pella Inc., Redding, CA). The disks were embedded in Epo-Thin epoxy resin (Buehler Ltd.). After curing for 18 hours, the surface of each epoxy cast was polished with wet SiC papers of decreasing abrasiveness (up to 1200 grit) and soft tissue with increasingly fine diamond suspension to a 0.05- m size (Buehler Ltd.). The specimens were sonicated in 100% ethanol for 5 minutes, demineralized i n 6 N HCl (Acros Organics USA,

Morris Plains, NJ) for 30 seconds, and deproteinized in 1% NaOCl for 10 minutes. The specimens were mounted on Al stubs and sputter- coated with Au-Pd in an E-5100 sputter-coater (Polaron Ltd., Watford, UK) at 40 mA for 90 seconds. Interfaces were observed under an S4700 Hitachi (Hitachi, Tokyo, Japan) field emission scanning electron mi- croscope (FESEM) at 4.0 to 5.0 kV.

Analysis of the Interface Using a Transmission Electron Microscope (TEM) Teeth were sectioned as in the previous group. Sticks with a cross- section of 1.5 1.5 mm were cut from the central area of the slice and immersed in 2.5% glutaraldehyde/2% paraformaldehyde in 0.1 M so- dium cacodylate buffer at pH 7.4 (Ted Pella Inc.) for 12 hours at 4°C. They were rinsed in 10 ml of 0.1 M sodium cacodylate buffer (Ted Pella Inc.) at pH 7.4 for 2 hours and postfixed with 2% osmium tetroxide in 0.1 M sodium cacodylate buffer (Ted Pella Inc.) for 1 hour followed by washing in 0.1 M sodium cacodylate for 1 hour. Specimens were then rinsed with deionized water four times and dehydrated in ascending grades of ethanol. The specimens were immersed in propylene oxide for 2 10 minutes and embedded in 50% propylene oxide/50% Med- Cast epoxy resin (Ted Pella Inc.) in a Pelco Infiltron rotator (Ted Pella Inc.) for 6 hours. The specimens were transferred to 100% epoxy resin for 12 hours to allow for resin infiltration. Specimens were mounted in molds filled with fresh MedCast epoxy resin and left in an incubator during 12 hours at 65°C. The resin-embedded blocks were sectioned in an ultra-microtome with a material-sciences diamond knife (Micro Star Technologies Inc., Huntsville, TX). The 85 10-nm-thick sections were mounted on 150-mesh nickel grids and stained with 2% uranyl acetate for 20 minutes and 3% lead citrate for 15 minutes. Observations were performed in a JEOL 1200 transmission electron microscope (TEM) (JEOL Ltd., Tokyo, Japan) at 80 kV.

FESEM Analysis of the Fitting Surface The roots were dissolved in 6N HCl for 48 hours at room temper- ature with one change and rinsed in distilled water for 2 4 minutes, followed by deproteinization in 2.6% NaOCl (The Clorox Co.) for 15 minutes. Specimens were then rinsed in distilled water for 2 4 min- utes. Specimens were processed for FESEM observation as described earlier.

Results

FESEM/TEM of the Interfaces

The adhesive materials ADH, EXC, and RS formed hybrid layers (HLs) but showed areas of interfacial separation. For ADH, the separa- tion occurred more frequently at the top of the HL ( Fig. 1 a ), whereas GP

showed areas of wide interfacial gaps ( Fig. 1 e , f ). Gaps in the total-etch adhesive EXC occurred more frequently between Multicore Flow and the adhesive layer, less frequently between the HL and the adhesive ( Fig.

1 c ). For RS, areas of cohesive separation in the sealant occurred at the

top of the HL ( Fig. 1 g ), with residual sealant left on the HL ( Fig. 1 h ).

Figure 1. FESEM (left) and TEM (right) microphotographs of the interfaces. (a ) FESEM micrograph of Adhese DC. High magnification ( 5,000) showing area of separation between the top of the HL and the adhesive material; (b ) TEM micrograph of Adhese DC ( 25,000) showing a partially calcified HL without any separation in this area; ( c ) FESEM micrograph of Excite DSC with an area of debonding between the adhesive and the composite MultiCore Flow and adhesive and HL. (d ) TEM micrograph of Excite DSC ( 7,500) showing a thick HL without signs of hydroxyapatite crystals. An area of debonding occurred above the HL with remaining particles of Multicore Flow embedded into the adhesive. (e ) FESEM micrograph of gutta-percha AH-26 showing a wide gap without any material infiltration into the dentinal tubules. (f ) TEM micrograph of gutta-percha AH-26 ( 10,000). The epoxy resin corresponds to an area of separation. (g ) FESEM micrograph of RealSeal sealer/Resilon points showing areas of debonding between the sealer and the HL. ( h ) TEM micrograph of RealSeal sealer/Resilon points ( 25,000). The epoxy resin corresponds to an area of debonding with residual sealant left on the HL. # Residual RealSeal sealant on the top of HL; *Areas of interfacial separation; HL, hybrid layer; D, dentin; MF, Multicore Flow composite; RT, resin tag; P, Resilon point; RS, RealSeal sealant; Ep, epoxy embedding resin; Gp, gutta-percha; AH, AH-26.

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Basic Research—Technology Figure 2. Composite FESEM of the fitting surface of Excite DSC and RealSeal with

Figure 2. Composite FESEM of the fitting surface of Excite DSC and RealSeal with Resilon points. The formation of resin tags into the dentinal tubules was much more frequent for Excite DSC (a ) than for RealSeal with Resilon points (b ). Note that the number of resin tags decreases in the apical third for Excite DSC and in the apical half for RealSeal/Resilon points.

RS and ADH resulted in a partially calcified HL ( Fig. 1 b ), whereas the HL of EXC contained no evidence of hydroxyapatite crystals ( Fig.

1 d ). The width of the HL was 0.3 to 0.4 m for ADH, 0.5 to 0.6 m for RS, and 4.0 to 7.1 m for EXC. GP did not form an HL.

FESEM of the Fitting Surface

FESEM of the fitting surfaces showed dentin resin tags at all levels for EXC, but less frequently in the apical third ( Fig. 2 ). Tags were much less frequent with ADH, especially in the apical third. For RS, resin tags were rare and virtually absent from the apical half. No resin tag exten- sions were formed with GP.

Discussion

The polymerization shrinkage creates stresses that may be of enough magnitude to result in detachment of the resin from the dentin of the canal walls, opening a pathway for bacterial leakage ( 21, 22 ). Bonding to root canal walls is mechanically unfavorable because of the higher C-factor that leads to an increase in shrinkage stresses ( 6 ). Despite the proven bonding efficiency of the control adhesives ADH and EXC to coronal and to root dentin ( 23–25 ), the unfavorable C-factor inside the canal may have led to high stresses that caused debonding. The resin did not have the opportunity to flow because of the con- strained space, which resulted in accumulation of stresses that develop within the polymerizing resin. A similar pattern has been found when bonding fiber posts to root canal dentin ( 26 ). Concerns have been raised regarding the alkaline hydrolysis susceptibility of Resilon points as compared to gutta-percha ( 27 ). The sealing ability of Resilon has also been questioned ( 17 ). Our findings are in agreement with the findings of Hiraishi et al. ( 28 ) who reported that the gaps in the Resilon group were also observed between the points and the sealer. This physical separation was not expected in view of the philosophy behind the monoblock concept. Sporadic air bubbles were observed in the body of the sealer (not

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shown). These air bubbles may have delayed the set of the sealer, which has been described as taking up to 1 week to fully set ( 29 ). This delay may have caused separation between the points and the sealer. The bond strengths of Resilon to a methacrylate-based resin, as that found in Resilon sealer, are 4 to 5 times lower than the bond strengths of a composite resin to the same sealer ( 28 ). Although this low magnitude of bond strengths with Resilon-based materials may cause some concern, other authors have reported a lack of correlation be- tween the sealing efficiency and the adhesive properties of root canal sealers ( 12 ). Factors such as shrinkage stresses and integrity of the attachment to the sealer may play a more important role in sealing than the respective adhesion strength. Nevertheless, the separation between the bottom of the RealSeal sealant and dentin, as observed in our study, would have caused leakage and potentially failure of the endodontic treatment in a clinical situation. The use of dual-cure resin-based materials to seal the root canal walls has been recommended ( 10, 13 ). Yet, the sealing efficiency of dual-cure resin-based cements is inferior to that of an epoxy-based sealer (13 ). Gap-free areas combined with interfacial gaps without resin tags have been associated with a Resilon-based material and with gutta-percha/AH-Plus ( 17 ). Despite the hybridization, a perfect seal of the root canal is difficult to achieve, which may be a result of the com- plexity of the substrate and the high C-factor. In the light of our findings, we must accept the null hypothesis; the dentin penetration and sealing ability of new root canal filling material is not superior to that of existing materials.

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