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J Am Dent Assoc, Vol 138, No 5, 634-640.
© 2007 American Dental Association
Essential Dental System, Inc.
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RESEARCH

JADA Continuing Education

Microleakage of self-etch primer/adhesives in endodontically treated teeth

Deniz Korasli, DDS, PhD, Fatmagül Ziraman, DDS, PhD, Perihan Ozyurt, DDS, PhD and S. Burcak Cehreli, DDS, PhD


   ABSTRACT
TOP
 ABSTRACT
MATERIALS AND METHODS
 RESULTS
 DISCUSSION
 CONCLUSION
 REFERENCES
 
Background. The authors evaluated the coronal marginal leakage of endodontically treated teeth bonded with four self-etching adhesives and one total-etch adhesive system.

Materials and Methods. The investigators prepared Class II cavities in 60 extracted human premolars. They performed conventional endodontic therapy using a resin-based sealer and gutta-percha points. They randomly assigned each tooth to a group receiving one of the following adhesives: Adper Prompt L-Pop (3M ESPE, Seefeld, Germany), Clearfil SE Bond (Kuraray, Osaka, Japan), FL Bond (Shofu, Kyoto, Japan), Single Bond (3M ESPE) or Xeno III (Dentsply De Trey, Konstanz, Germany). They restored all teeth with resin-based composite material (Z250, 3M ESPE). Specimens underwent thermocycling and dye penetration and were sectioned longitudinally. The authors photographed the sections under a stereomicroscope. They transferred the images to an IBM-compatible personal computer for quantitative assessment of dye penetration using image analysis software. They analyzed data by means of Kruskal-Wallis and Mann-Whitney U tests (P = .05) and evaluated two specimens from each group under scanning electron microscopy.

Results. None of the tested self-etch adhesives completely eliminated microleakage. Dye leakage was restricted to the coronal cavity walls; it did not migrate toward the pulp chamber or toward the root canal. Single Bond and Clearfil SE Bond showed significantly lower dye penetration values at occlusal and gingival margins.

Conclusions. The coronal sealing performance of the tested self-etch adhesive systems in endodontically treated teeth was material-dependent. The use of Clearfil SE Bond in such teeth can help achieve a marginal seal comparable to that achieved with Single Bond.

Key Words: Self-etch adhesive; microleakage; endodontically treated teeth; total-etch adhesive

Abbreviations: SEM: Scanning electron microscopy

Despite advances in endodontic materials and techniques that aim to achieve a totally sealed root canal system, root canal fillings demonstrate microleakage over time. When the coronal portion of the root canal is exposed to the oral environment, the obturated canal becomes a potential route by which microorganisms can gain access to peri-apical tissues.1 When the coronal portion is not sealed, endotoxin from Actinobacillus actinomycetem-comitans can pass through obturated root canals within 20 days,2 and saliva can reach the apical region through an obturated canal in as quickly as three days.3 One study evaluating the relationship between quality of the coronal restoration and radiographic success of endodontically treated teeth has shown that a good coronal seal results in significantly less occurrence of periradicular inflammation.4 The technical quality of the coronal restoration, thus, may be significantly more important for long-term apical periodontal health than is the technical quality of the endodontic treatment.4

Various techniques and materials are used for the final coronal restoration of endodontically treated teeth. Besides achievement of a hermetic marginal seal, these materials and techniques are used to reinforce the residual tooth structure, another major consideration in long-term clinical success. Previously, it was believed that biological changes occured in teeth after endodontic treatment, rendering them more brittle and susceptible to failure.5,6 Thus, endodontically treated teeth traditionally have been treated with full-coverage restorations, mostly in conjunction with a core and/or a dowel in the belief that those devices further reinforced the teeth.7 This often has led to the sacrifice of remaining sound tooth structure for the preparation of a traditional cast restoration. It has been shown by some investigators that a core, a dowel or pins weaken the tooth rather than reinforce it.8–10 Moreover, recent work has demonstrated that it is the loss of tooth bulk and sound dentin that causes the reduction in the relative stiffness of the tooth.11–15

Today, the possibility of direct restoration of nonvital teeth with resin-based composites has increased owing to the development of more reliable bioadhesive systems. To improve the tooth’s fracture resistance and longevity, researchers have advocated the satisfactory use of adhesive restorative systems for endodontically treated teeth.13,15,16 Nevertheless, endodontically treated teeth may offer different conditions for bonding. For instance, depending on the tooth’s status when bonding is performed, exposure of root-treated dentin to various disinfectant or irrigation solutions such as sodium hypochlorite may influence the hybridization quality of intraradicular dentin.17 Moreover, bonding to the pulp chamber may be different from bonding to coronal dentin.15 Because the volume of the restoration is larger in endodontically treated teeth, more resin increments are necessary to fill the cavity preparation. Finally, cusps lose their pulp chamber’s roof support and may flex owing to shrinkage stresses. All these factors may affect the marginal quality of bonded restorations in endodontically treated teeth.

Numerous commercial bonding systems are available under two simplified approaches: "total-etch" (also termed "etch and rinse") and "self-etch" adhesives. For total-etch bonding systems that use phosphoric acid etching of enamel and dentin before bonding, it has been considered that the demineralized and uninfiltrated dentin zone becomes the weak point of the bond owing to hydrolytic degradation of collagen over time.18,19 Although the reduction or absence of demineralized dentin for the simplified so-called "self-etching" systems was believed primarily to prevent hydrolytic degradation of bonded structures, it recently has been shown that hydrolysis of collagen may well take place in the long term.20 This is clinically significant, because the degradation between resin-dentin bonds may enable access for microleakage, thus resulting in failure of the coronal seal as well as loss of micromechanical support for the coronal tooth structure.

Although a multitude of publications report microleakage patterns after adhesive procedures in vital teeth, there is a scarcity of published data regarding those in endodontically treated teeth and none specifically dealing with self-etching primer/adhesive systems in endodontically treated teeth. Thus, the aim of our study was to evaluate the in vitro coronal (occlusal and cervical) microleakage of endodontically treated teeth bonded with self-etch adhesive systems.


   MATERIALS AND METHODS
TOP
 ABSTRACT
 MATERIALS AND METHODS
RESULTS
 DISCUSSION
 CONCLUSION
 REFERENCES
 
Specimen preparation. For the study, we selected 60 human mandibular premolars with straight root canals and fully developed apexes extracted for orthodontic reasons. After débriding tooth surfaces with a hand-scaling instrument and cleaning the teeth with a rubber cup and a slurry of pumice, we stored them in saline solution for up to one month at 4 C.

One operator (D.K.) prepared standardized Class II mesioocclusal (MO) cavities (buccolingual width of 3 millimeters on the occlusal and gingival sides) with a no. 245 tungsten carbide bur in a high-speed handpiece under copious water spray. She finished the gingival margin approximately 1 mm below the cementoenamel junction in dentin, as verified subsequently under a stereomicroscope at x10 magnification. No bevels were added at any margin of the preparation.

On removal of the roof of the pulp chamber to gain access to the root canals, the operator removed the pulp tissue with a barbed broach (no. 25, Dentsply-Maillefer, Ballaigues, Switzerland), established working length 1.0 mm short of the apical foramina, and instrumented the root canals to the same file size (no. 55 file, Dentsply-Maillefer) using the step-back technique. She irrigated the root canals with 5.25 percent sodium hypochlorite between uses of each file size. On completion of the instrumentation, she obturated root canals with a resin-based sealer (AH Plus, Dentsply De Trey, Konstanz, Germany) and gutta-percha points (Dentsply-Maillefer) in conjunction with a lateral condensation technique. The operator sealed coronal root canal openings with a thin layer of conventional glass ionomer cement, and we randomly assigned teeth to one of the following groups (n = 12):

– group 1: Adper Prompt L-Pop (3M ESPE, Seefeld, Germany);
– group 2: Xeno III (Dentsply De Trey);
– group 3: Clearfil SE Bond (Kuraray, Osaka, Japan);
– group 4: FL Bond (Shofu, Kyoto, Japan);
– group 5: Single Bond (3M ESPE).

The operator applied all adhesives in strict accordance with manufacturers’ instructions.

The operator restored all samples incrementally with resin-based composite (Z250, 3M ESPE) using a visible light curing unit (Optilux 401, 40 seconds/1-mm increment, Kerr, Danbury, Conn.). A new curing unit was used to ensure complete polymerization. The restorations were polished with fine and superfine Sof-Lex Disks (3M Dental Products, St. Paul, Minn.). After 24 hours’ storage in water at 37 C, all teeth were subjected to 500 temperature cycles (5 ± 2 to 55 ± 2 C, dwell time 30 seconds). The operator sealed the root apexes with sticky wax to prevent dye penetration. She coated the samples with two consecutive layers of nail varnish up to 1 mm from the restoration margins. She immersed the samples in 0.5 percent basic fuchsin solution (Wako Pure Chemical Industry, Osaka, Japan) for 24 hours. Thereafter, she rinsed samples thoroughly under tap water, air-dried them and embedded them in a phenolic ring with epoxy resin (Struers, Copenhagen, Denmark). Four parallel longitudinal sections were made through the resin restorations using a low-speed water-cooled diamond saw (IsoMet, Buehler, Lake Bluff, Ill.) in the mesiodistal direction.

Microleakage evaluation. For each specimen, dye penetration along the occlusal and gingival margins on each of the four sectioned surfaces was digitally photographed at x20 (resolution of 1,280 x 1,024 dots per inch) under a stereomicroscope (Olympus, Tokyo, Japan) and the data were transferred to a personal computer. On each section, one of the authors (S.B.C.) measured the staining along both occlusal and gingival restoration interfaces using image analysis software (Scion Image for Windows, Version 4.0.2, Scion, Frederick, Md.). The differences in the amount of dye penetration in the occlusal and gingival margins were evaluated statistically using Kruskal-Wallis and Mann-Whitney U tests, with significance set at P = .05.

Scanning electron microscopy (SEM) evaluation. For each group, two of the authors (D.K. and S.B.C.) prepared and sectioned two teeth in the same manner described earlier to evaluate the tooth-adhesive interface under SEM. They first exposed the sections to hydrogen chloride for 15 seconds followed by 1 percent sodium hypochlorite for 10 minutes, and then dehydrated them in ascending grades of ethanol (30, 50 and 95 percent for 30 minutes each, and 100 percent for 60 minutes). After the final ethanol bath, they dried the specimens by immersion in hexamethyl-disilazane (HMDS, Electron Microscopy Sciences, Hatfield, Pa.) for 30 minutes, placed them on filter paper inside a covered glass vial and kept them in a vacuum for 24 hours. Subsequently, they sputter-coated the specimens with gold-palladium (Balzers-SCd 050 sputter coater, Balzers, Liechtenstein) for observation with the use of a scanning electron microscope (JSM-6400 V, JEOL, Tokyo) at 20 kilovolts of accelerating voltage.


   RESULTS
TOP
 ABSTRACT
 MATERIALS AND METHODS
 RESULTS
DISCUSSION
 CONCLUSION
 REFERENCES
 
Microleakage test. The tableGo presents dye penetration values demonstrated by the test materials. None of the tested adhesive systems completely eliminated microleakage at occlusal and gingival margins. For all adhesives, the extent of dye penetration in occlusal and gingival restoration margins did not differ significantly (P > .05). The lowest occlusal microleakage values were attained in samples bonded with Single Bond and Clearfil SE Bond. There was no significant difference in microleakage between these two adhesive systems (P > .05, Mann-Whitney U test).


View this table:
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  		TABLE Amount of occlusal and gingival dye penetration produced by total-etch and self-etch adhesives.

 
Clearfil SE Bond and Single Bond demonstrated significantly lower microleakage than did Xeno III, Adper Prompt L-Pop and FL Bond (P < .05). Among all tested adhesive systems, FL Bond yielded the highest microleakage values. However, there was no statistically significant difference between the microleakage values of Xeno III, Adper Prompt L-Pop and FL Bond (P > .05, Mann-Whitney U test).

As happened with the occlusal margins, the best gingival seal was attained with Clearfil SE Bond and Single Bond. The microleakage scores of both adhesive systems did not differ significantly (P > .05, Mann-Whitney U test). Clearfil SE Bond yielded a marginal seal significantly better than that of the other tested self-etch adhesives (P < .05). Again, there was no statistically significant difference between the microleakage values of Xeno III, Adper Prompt L-Pop and FL Bond (P > .05, Mann-Whitney U test).

SEM evaluation. Figures 1Go through 5GoGoGoGo show the SEM findings. Xeno III created a continuous hybrid layer 2 to 3 micrometers thick. The submicron hiati beneath this layer did not suggest a separation or artifact caused by fixation or SEM procedures (Figure 1Go). Resin tags were present in only a few tubules. Clearfil SE Bond created a continuous hybrid layer 2 to 5 µm thick. Resin tags were present, uniformly extending deep into dentin. Among the resin tags, thin lateral hybridizations could be detected (Figure 2Go). Adper Prompt L-Pop created a uniform hybrid layer 4 to 5 µm thick. We observed a pronounced resin tag formation and complete tubular seal in this group (Figure 3Go). Morphologically, Single Bond created the most uniform hybrid layer among the tested adhesives; it was 5 to 7 µm thick without any visible separation or gap. A uniform, continuous resin tag formation could be observed through deep dentin, with well-defined lateral tubule hybridization (Figure 4Go). FL Bond created the thinnest hybrid layer (1–2 µm) among the tested adhesives. The hybrid layer was partly separated from dentin. Most of the tubules showed no resin tag formation, and the present tags were markedly narrow (Figure 5Go).


Figure 1
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  		Figure 1. Scanning electron microscopic image of dentin–Xeno III (Dentsply DeTrey, Konstanz, Germany) adhesive interface. The sub-micron hiati (arrows) are evident.

 

Figure 2
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  		Figure 2. A typical view of hybrid layer formation in Clearfil SE Bond (Kuraray, Osaka, Japan). A thin, continuous hybrid layer is evident.

 

Figure 3
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  		Figure 3. Scanning electron microscopic image of dentin–Adper Prompt L-Pop (3M ESPE, Seefeld, Germany) adhesive interface. A thick, uniform hybrid layer is visible.

 

Figure 4
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  		Figure 4. Scanning electron microscopic image of dentin–Single Bond (3M ESPE, Seefeld, Germany) adhesive interface. A uniform, continuous hybrid layer formation associated with lateral tubule hybridizations (arrows) is evident.

 

Figure 5
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  		Figure 5. Hybrid layer formation in FL Bond (Shofu, Kyoto, Japan). An extremely thin adhesive interface with narrow resin tags was typical.

 

   DISCUSSION
TOP
 ABSTRACT
 MATERIALS AND METHODS
 RESULTS
 DISCUSSION
CONCLUSION
 REFERENCES
 
The sealing performance of adhesive resins is affected by cavity configuration (C-factor), dimensional changes of the restorative material (for example, polymerization shrinkage or thermal/ hygroscopic expansion) and the bonding capacity of the adhesive resins.21 In our study, we made every attempt to produce an identical cavity size to avoid the effect of cavity configuration. It should be noted, however, that the anatomy of the pulp chamber dictated the final shape of the endodontic access cavity, which may have caused small variations. Also, different adhesives were bonded to one resin-based composite material so as to discard changes that may arise from use of specific or nonspecific restorative systems.22

Microleakage tests are useful methods to evaluate the sealing performance of adhesive systems. Among different methods used, dye penetration measurements on sections of restored teeth is the technique most commonly used. In our study, we made four sections through each restoration to increase the reliability of our measurements.23 We combined this technique with image analysis to obtain quantitative results instead of a conventional subjective scoring. A relative merit of this objective approach compared with a subjective scoring system was to discard the need for scoring by separate evaluators and for consensus scoring in borderline cases, as well as statistical procedures with regard to interexaminer reliability.

We based the number of thermal cycles used in our study on the work of Crim and Garcia-Godoy,24 who reported that the degree of dye penetration is not significantly different for 100 versus 1,500 cycles. Further refinement in the technique used herein might include thermocycling in dye solution rather than in water. Although load cycling could be considered another possible methodological enhancement from a biomechanical standpoint, Mitsui and colleagues25 demonstrated that mechanical load cycling had no effect on the microleakage of either self-etch or total-etch adhesives.

Self-etch adhesive systems have become increasingly popular in the last decade. The combination of etchant and primer into one system is advantageous in that it reduces the application time and technique-related sensitivity.26 On the other hand, there is an ongoing debate regarding the efficacy of bonding to enamel with self-etch adhesive systems.27 Some authors support the manufacturers’ recommendations that the adjunctive use of phosphoric acid etching is necessary when bonding to uncut enamel,27 while others argue that the bond strengths of self-etch adhesives are equal to the bond strength of total-etch adhesives to unground enamel.28 To date, no correlation has been established between micro-leakage scores and bond strengths of dental adhesive systems.29 In our study, the sealing performance of Clearfil SE Bond was comparable with that of the total-etch adhesive, Single Bond, on enamel margins. These findings are consistent with previous laboratory data.30,31

Contemporary self-etch adhesive systems can be categorized as "mild," "moderate" and "aggressive," depending on the acid dissociation constants (known as "pKa values") of the acidic resin monomers used and the concentration of the monomers present in the adhesives.26,32 The bonding mechanism of mild self-etch adhesives to dentin is characterized by submicron hybrid layers associated with less pronounced resin tag formation.32 On the other hand, strong self-etch adhesives have been shown to produce hybrid layers that are similar morphologically to those typically produced by total-etch adhesives. Consequently, the mechanism of bonding strong self-etch adhesives to dentin is more like that of the total-etch adhesives, since almost the entire hydroxyapatite content is removed from superficial collagen and, thus, any chemical interaction between hydroxyapatite and functional monomers is avoided.26,32 In our study, the thick hybrid layer and pronounced resin tag formation observed in Adper Prompt L-Pop–treated samples corroborates the above-mentioned mechanism. By contrast, the mild self-etch adhesives Xeno III and Clearfil SE Bond created a thin hybrid layer. The morphological features of the hybrid layer produced by Clearfil SE Bond are in line with the findings that Osorio and colleagues31 obtained with nonobturated extracted teeth.

FL Bond contains 4-acryloxyethyltrimellitic acid (4-AET) as an adhesion-promoting monomer. A self-etch primer containing 4-AET is able to interact with both hydroxyapatite and collagen fibrils in dentin substrates, into which the monomer penetrates. SEM and X-ray micro-analysis studies on bonded interfaces of a self-etching primer containing 4-AET have demonstrated a considerable amount of calcium entrapped in the etched dentin.33 The ionized carboxyl groups in the 4-AET monomer may combine with the calcium of the original and remnant apatite crystallites within the hybrid layer to form insoluble salts.33 It has been demonstrated that an adhesive resin formulation that contains 4-AET may bond to dentin via ionic interaction.34 This may explain the thin hybrid layer and absence of resin tags that we observed in FL Bond–treated resin-dentin interfaces. On the other hand, Clearfil SE Bond contains the functional monomer 10-methacryloxyloxydecyl dihydrogen phosphate (10-MDP), which has two hydroxyl groups that also may bind to calcium.35 Recently, Yoshida and colleagues36 reported that MDP tightly adheres to hydroxyapatite and that its calcium salt hardly dissolved in water. Moreover, 10-MDP causes minimal dissolution of smear plugs and limited opening of tubules, reducing dentin permeability.37 10-MDP also facilitates penetration, impregnation, polymerization and entanglement of monomers with demineralized dentin to form a relatively thick hybrid layer.38 The lower dye penetration observed in the samples that were bonded with Clearfil SE Bond could be attributed to the difference in chemical compositions of the self-etch adhesives.36 Further studies are required to clarify the adhesive performance of the functional monomers present in self-etch systems.


   CONCLUSION
TOP
 ABSTRACT
 MATERIALS AND METHODS
 RESULTS
 DISCUSSION
 CONCLUSION
REFERENCES
 
The use of self-etch adhesives in conjunction with resin-based composites in the final coronal restoration of endodontically treated teeth may help reduce microleakage, though results obtained within the experimental conditions of our study clearly show that the sealing performance was material-dependent. Clearfil SE Bond was the only adhesive material that performed equivalently to the sealing performance of the total-etch adhesive, Single Bond. Dye leakage with Clearfil and Single Bond was restricted to the cavity walls in the coronal portion, and no dye was seen migrating toward the pulp chamber or toward the root canal. Thus, more laboratory studies using aging techniques (for example, long-term water storage, load and thermal cycling, and so forth) are required to assess the extent of dye migration, as well as the effect of placing glass-ionomer cement sealers beneath resin-based composite restorations.


   FOOTNOTES
 

Dr. Korasli is a research assistant, Ankara University Faculty of Dentistry, Department of Endodontics, Besevler, 06500, Ankara, Turkey, e-mail "dkorasli{at}yahoo.com". Address reprint requests to Dr. Korasli.


Dr. Ziraman is a professor, Ankara University Faculty of Dentistry, Department of Endodontics, Turkey.


Dr. Ozyurt is an associate professor, Ankara University Faculty of Dentistry, Department of Endodontics, Turkey.


Dr. Cehreli is a research associate, Baskent University Faculty of Dentistry, Department of Pediatric Dentistry, Ankara, Turkey.


   REFERENCES
TOP
 ABSTRACT
 MATERIALS AND METHODS
 RESULTS
 DISCUSSION
 CONCLUSION
 REFERENCES
 

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