jindiansocpedodprevdent302133-1475557_040555

133JOURNAL OF INDIAN SOCIETY OF PEDODONTICS AND PREVENTIVE DENTISTRY | Apr - Jun 2012 | Issue 2 | Vol 30 |

Original article

Self etching adhesive on intact enamel

Devarasa GM, Subba Reddy VV, Chaitra NL1

Department of Pedodontics and Preventive Dentistry, College of Dental Sciences, Davangere, Karnataka, 1Department of Pedodontics and Preventive Dentistry, Kothiwal Dental College and Research centre, Kanth Road, Moradabad, Uttar Pradesh, India

Correspondence: Dr. G. M. Devarasa, Senior Lecturer, Department of Pedodontics and Preventive Dentistry, College of Dental Sciences, Pavilion Road, Davangere-577004, Karnataka, India. E-mail: [email protected]

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DOI: 10.4103/0970-4388.99987

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Abstract

Background and Objective: to analyze the poor performance of self-etch adhesives on intact enamel. Materials and Methods: labial surfaces of 20 caries free permanent upper central and lateral incisors were cleaned, sectioned of their roots. All specimens were mounted on acrylic block and divided randomly into two groups. In one group the application of self-etch adhesive was carried as per manufacturer’s instructions, composite cylinders were built, whereas in the other group, 37% phosphoric acid was applied before the application of self-etching adhesives. Then the resin tags were analyzed using the scanning electron microscope. Results: showed that when phosphoric acid was used, there was significant increase in the depth of penetration of resin tags. Conclusion: the results indicate that out of both treatment groups, pre-etching the intact enamel with 37% phosphoric acid resulted in the formation of longer resin tags and higher depth of penetration of resin tags of the Clearfil SE bond, which might have resulted in attaining higher bond strength of the Clearfil SE bond to intact enamel.

Key words

Permanent maxillary incisors, phosphoric acid, pre-etching, resin tag, self-etch adhesives, shear bond strength

Introduction

The introduction of enamel bonding leads to an increasing demand for restorative and nonrestorative esthetic treatments have transformed the practice of operative dentistry.

The introduction of reliable[1] adhesive restorative materials have substantially reduced the need for extensive tooth preparations since the introduction of acid etching by Buonocore in 1955. Although the bond strengths of adhesive systems were satisfactory, simplified adhesive systems were developed in order to reduce the number of steps during the bonding procedures.

The first simplification was the fifth generation of bonding agents, systems in which the primer and the adhesive were mixed together and supplied as a single system.

Two systems even simpler to use were developed, one consisting of an acidic primer and a bonding resin is referred to as a sixth-generation adhesive and another in which the etchant, primer, and adhesive are combined into one single delivery system marketed as seventh generation of adhesive systems.

Though the self-etching primers have been reported to produce high bond strength to dentin, only limited evidence exists reporting that self-etching primers can be used for bonding composites to intact enamel.

The scanning electron microscopy helps us in the assessment of bonding efficacy of the bonding agents by examining the resin tag penetration depth.

Materials and Methods

A total of 20 teeth were divided into two groups of 10

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Devarasa, et al.: Pre etch before self etch?

134 JOURNAL OF INDIAN SOCIETY OF PEDODONTICS AND PREVENTIVE DENTISTRY | Apr - Jun 2012 | Issue 2 | Vol 30 |

samples each. The samples were cleaned and scaled using ultrasonic scaling unit, the roots were sectioned and the crowns were stored in distilled water. Routine prophylactic procedure was carried out with rubber cup and aqueous slurry of pumice for all the teeth before they were treated.

Samples were mounted horizontally on acrylic resin blocks. Teeth were mounted by keeping the labial surface exposed.

Bonding agent was used as per manufacturers instructionsClearfil SEPrimer was applied on to the enamel surface and left for 15 s, followed by gentle air drying; application of adhesive and left for 10 s, followed by gentle air drying and light curing for 10 s.

Bonding protocol foreach groupGroup A: Self-etch adhesive was applied over intact labial enamel as per manufacturer’s instructions.

Group B: Labial enamel was etched with 35% phosphoric acid as per manufacturer’s instructions. Self-etch adhesive was then used as like group A.

For group A and B, 1 mm thick layer of composite was placed over the bonded enamel surface and cured for 40 s using Halogen light curing unit (3M ESPE) and the specimens were store in deionized distilled water at 37°C for 24 h.

Resin tag analysisThe resin tag analysis was done using the scanning electron microscope. The specimens from group A and B were used for resin tag analysis.[Figure 1] The Crowns were sectioned longitudinally in a labiolingual direction to a thickness of 1 mm, using a hard tissue microtome. All specimens were cleaned in distilled water with ultrasonic agitation for 30 min and gently air dried. They were fixed to SEM stubs, gold sputtered [Figure 2] for 10 min and the resin enamel interface of the specimens were examined under the SEM machine at an optical zoom of 2000× for the evaluation of resin tags.[Figures 3,4]

Statistical analysisIntergroup comparisons of the results of resin tags were analyzed by Mann–Whitney U test. The mean values(ΔE*)werecalculatedforeachgroup.Thelevelof significance for all the tests was chosen as P < 0.001

Results were expressed as mean ± SD. Mann Whitney

U analysis was used for groupwise comparisons.

The P value was calculated for statistical significance.

Results (Resin Tags)

This in vitro study was carried out to evaluate and compare the resin tags of self-etch adhesives formed on intact enamel with and without pre etching with 37% phosphoric acid.

The samples after completing the bonding procedures were sectioned using hard-tissue microtome, gold sputtered, and examined under the scanning electron microscope.

The resin tag analysis was done by measuring the depth of the penetration of the resin tags into the enamel in micrometers.

Table 1 shows the values of the different samples of the group A and B regarding their range, mean, median values of the resin tag penetration depths in the micrometer.

Group A: The range of depth of the penetration of the resin tags into the enamel in micrometers in group A was 0-8.14 mm with a median depth of penetration of 4.07 mm with a mean of 3.67 mm.

Group B: the range of depth of the penetration of the resin tags into the enamel in micrometers in group B was 9.3-27.9 mm with a median depth of penetration of 18.13 mm with a mean of 16.9 mm.

Table 2 shows the comparison of the two groups regarding their Mean ± SD of the resin tag penetration depths in micrometer.

The Mean ± SD of group A is 3.67 ± 2.85 mm

The Mean ± SD of group B is 16.9 ± 5.48 mm

Inter group comparisonsAt the end of treatment the improvement in resin tag penetration depth of self-etch adhesive on intact enamel on pretreatment with 37% phosphoric acid was 95.4%.

The results showed that Group A demonstrated lower resin tag penetration depths than Group B exhibiting statistically significant difference with P value of <0.001 [Table 2].





Discussion

The enamel bonding potency of self-etch adhesives over intact enamel is highly questioned mainly due to its decreased efficacy in creating a definitive etch pattern.

A bonding agent for giving better bond strength on a dental substrate has to form a uniform well-penetrating resin tags within the dental substrate. Bonding to the intact surface of enamel is important to prevent marginal leakage, and provide maximum bond strength. In most studies investigators flattened enamel surfaces using silicon carbide prior to application of adhesives. So an in vitro study was conducted to evaluate the resin tag formation of self-etch adhesives over intact enamel with and without pre-etching with 37% phosphoric acid.

“In this study, the investigations were carried out on intact enamel that is very important for certain procedures. The results of this study suggested that adequate bonding to intact enamel with self-etch adhesives alone cannot be achieved and will require additional phosphoric acid etching for 15 s at a concentration of 37% is used.”

The intact enamel surface is hyperminerlized and contains more fluoride than ground enamel. It is reported that after teeth eruption, changes occur in the outermost enamel. Saturated calcium phosphate might hyper mineralize the enamel, and the fluoride ions might convert the hydroxyapatite into fluorapatite. Thick prismless enamel layer may prevent the permeation of self-etching primers and bonding agents and thus leaving some areas partially unetched, which may result in formation of shorter and poorly defined resin tags. Phosphoric acid etching removes the outermost enamel and there by resulting in formation of longer resin tags and there by increasing the bond strength.[2]

The aggressive etching effect of phosphoric acid on the enamel surface overcomes the difficulty of conditioning of intact or unprepared surfaces. The formation of a deep etching pattern leads to similar bond strength, when the adhesives are applied in both enamel surfaces.[3]

Self-etching systems contain acidic monomers based on esters from phosphoric acid, carboxylic acid, or their derivatives. Their etching efficacy and bonding formation depends on the type of acidic monomer, pH of adhesive solution, etching time, and application method. Acidic monomers are responsible for etching the dental substrates, whereas methacrylate components, such as HEMA, are available for monomer infiltration and polymerization of the bonding agent.[4]

Marina Di Francescantonio reported that the pH values of all self-etching systems were higher than phosphoric acid. In general, the demineralization effects of these systems are proportional to the acidity of the acidic primers or self-etching adhesive solutions. The self-etching primers are less aggressive than phosphoric acid etchants, and do not form a proper and defined acid etching pattern and the conditioning effects are also reduced in intact enamel surfaces, except for the Tyrian SPE primer, which is considered a strong self-etching adhesive with a very low pH (0.5). The etching pattern formed on both ground and intact enamel surfaces is similar to that promoted by phosphoric acid. Moderate self-etch systems include Optibond Solo Plus SE and Xeno III adhesives with pH 1.4 and 1.5, respectively, while Unifil Bond (pH 2.2) and One-Up Bond F (pH 2.6) systems are considered mild. The bonding mechanism of these self-etching systems to enamel is based on nanoretentive interlocking between crystallites and adhesive resin. These morphological features of the resin-enamel bonds are different from that formed with the etch and rinse adhesive systems. This thin hybridized complex of resin formed in enamel, produced by self-etchings without the usual micrometer-size resin tags can be responsible for lower bond strengths presented by some self-etching systems and the questionable effectiveness of this type of dental adhesives on enamel surfaces. Optibond Solo Plus SE and One-Up Bond F systems performed better on prepared enamel than on unprepared enamel.

Table 1: Range, mean and median of resin tag penetration depths in micrometer of group A and BStudy Group (n = 10) Range (micrometer) Mean (micrometer) Median (micrometer) SDGroup A 0-8.14 3.67 4.07 ±2.85Group B 9.3-27.9 16.90 18.13 ±5.48

Table 2: Mean and standard deviation of resin tag penetration depths in micrometer of group A and BStudy group (n = 10)

Mean ± SD Z* Value Significance

Group A 3.67 ± 2.85 3.75 P < 0.001 Highly SignificantGroup B 16.90 ± 5.48*Mann Whitney U test





Although Optibond Solo Plus SE primer presents low pH (1.5), it did not bond to unprepared enamel, leading to pretesting debonding in all specimens.[4]

For One-Up Bond F, SEM analysis of treated enamel surfaces with the adhesive solution revealed an extremely mild etching pattern, regardless of the surface preparation. This probably occurred due to the very mild pH (2.6) of the system, which would not provide adequate demineralization for infiltration of monomers. This pattern helps us to explain the bond strength results, which were lower when compared to the ground surface. The higher bond strengths to the SiC-prepared surface can be attributed to the roughness of the surface that facilitates the activity of the self-etching adhesive to form a defined etching pattern for infiltration of adhesive resin.[4]

The removal of superficial, aprismatic layer, by wet-grinding with 600-grit SiC paper improves the etching effects. As the morphological structure and composition of the intact peripheral surface of the enamel is different from that of the middle enamel layer, these differences can be favorable for etching effects in the subenamel surface.

For Optibond Solo Plus SE and One-Up Bond F systems, the enamel surface preparation resulted in higher bond strength. Enamel preparation using 600-grit SiC paper is unlikely to affect resin enamel bond strengths.[4]

Pashley and Tay reported that the efficacy of self-etching primers in intact enamel does not depend solely upon their etching aggressiveness, but on monomeric composition of each material. It is also possible that the low enamel bond strengths might be caused by the high amount of unpolymerized acidic monomers remaining after curing.[3]

Self-etching primers contain acidic monomer and water, which decalcifies the inorganic parts of a tooth but generally its acidity is weak. The acidic portion of the primer is neutralized by the calcium and phosphate ions released during decalcification of enamel, and thereby the decalcification process of enamel is ceased. SEM analysis has revealed that phosphoric acid etching prior to application of the self etch adhesives, created a deeper etching pattern and thicker tag-like resin penetration than priming alone.[5]

SEPs have demonstrated a shallower etch pattern.

This might be simply because of a poorer penetration of the SEP into the enamel porosities or the result of interference from mineral precipitates on the enamel surface that mask the etch pattern. Because the acidic primer is not rinsed off, phosphorous and calcium ions released from the hydroxyapatite crystal dissolution remain suspended in the primer solution. With the SEPs, the ionic precipitate remains embedded in the resin after polymerization.[6]

Kanemura et al. concluded stating that the phosphoric acid etching produced good resin adhesion to ground and intact enamel, whereas the self-etch adhesives clearfil liner bond II, Tokuso mac bond II produced good bonds on ground enamel, but had lower bond strength on intact enamel. The causes were attributed to the hypermineralized intact enamel with higher fluoride content and a thick layer of the prismless layer on intact enamel. It was also seen that the resin tags were shorter, poorly defined, and structurally incomplete. Phosphoric acid etching removes the outermost enamel layer and creates microirregularities and thereby results in good penetration of the resin etched intact enamel.[2]

Miguez PA study concluded saying that acid etching prior to application of self-etching primer clearfil SE bond, produced higher bond strength to enamel than self-etching priming only. The self-etch primer caused less demineralization of enamel compared to the total etch systems. The shallower pattern of demineralization is due to difficulty in penetration of the primer into enamel and due to the precipitation of minerals on enamel that might modify the depth of demineralization.[7]

Perdigao reported that, Single Bond, the total-etch adhesive, resulted in statistically higher microtensile bond strength than any of the other adhesives regardless of the enamel preparation. All self-etching adhesives resulted in higher microtensile bond strength when enamel was roughened than when enamel was left unprepared. The field-emission scanning electron microscope revealed a deep interprismatic etching pattern for the total-etch adhesive, whereas the self-etching systems resulted in an etching pattern ranging from absent to moderate.[8]

Marina Rotta concluded that all self-etching adhesives showed lower uTBS values than those obtained in phosphoric acid groups. Lower bond strength was mainly attributed to the low acidity of self-etch





adhesives and less distinct etch pattern exhibited when the enamel was conditioned with self-etching adhesive. CSE exhibited the mildest etching pattern. All self-etching adhesives applied after phosphoric acid exhibited a more retentive etching pattern. It was concluded that the bond strength values of low-pH self-etching adhesives can be improved by the adjunctive use of phosphoric acid or replacement of the bonding resin.[9]

Nasr stated that the demineralizing capacity of a product depends on such factors as its pH (for strong acids) or pKa (for weaker acids), its chelating ability, or the solubility of its calcium salts and of the duration of application. The strongest demineralizations are yet

less than the reference value observed with phosphoric acid.[10]

Pisol Senawongse compared three commercially available adhesive materials single bond (total etch), Clearfil SE Bond (two step self etch), One-Up Bond (one step self-etch) for their microshear bond strength on intact and ground enamel. The results showed that the two self-etching bonding agents showed lower bond strength than the total etching system on intact enamel, where as there was no significant differences in the bond strength on ground enamel. The resin tags in the single bond group revealed abundant longer resin tags on both intact and ground enamel. In the case of self-etch adhesives, short resin tags were seen in case of ground enamel, whereas on intact enamel, the short resin tags were rarely seen.[11]

Further studies testing these materials in vivo are warranted to determine whether the amount of bonding is the same as the in vitro study, is clinically relevant.

Conclusion

Within the limitations of this study conducted and the results obtained, it can be concluded that

Figure 1: Labilolingual crossections For SEM

Figure 2: SEM Stubs and gold sputtered samples

Figure 3: Resin tags of self-etch adhesive without pre etching

Figure 4: Resin tags of self-etch adhesive with pre etching

Figure 5: Resin tag penetration depth





“Out of both treatment groups, pre etching the intact enamel with 37% phosphoric acid resulted in longer resin tags (higher depth of penetration of resin tags) and this can be the reason of low bond strength of self etch adhesives on intact enamel.”

References

1. Roberson TM, Heymann HO, Swift EJ. Fundamentals of dental bonding: Sturdevent’s Art and Science of Operative Dentistry.Mosby 5th ed. 2006. p. 243-79.

2. Kanemura N, Sano H, Tagami J. Tensile bond strength to and SEM evaluation of ground and intact enamel surfaces. J Dent 1999;27:523-30.

3. Pashley DH, Tay FR. Aggressiveness of contemporary self-etching adhesives. Part 2: Etching effects on unground enamel. Dent Mater 2001;17:430-44.

4. di Francescantonio M, de Oliveira MT, Shinohara MS, Ambrosano GMB, Giannini M. Bond strength evaluation of self-etch and total-etch adhesive systems on intact and ground human enamel. Braz J Oral Sci 2007;6:1462-6.

5. Torii Y, Itou K, Nishitani Y, Ishikawa K, Suzuki K. Effect of phosphoric acid etching prior to self etching primer application on adhesion of resin composite to enamel and dentin. Am J Dent 2002;15:305-8.

6. Cal-Neto JP, Miguel JA. Scanning electron microscopy evaluation of the bonding mechanism of a self-etching primer on enamel. Angle Orthod 2006;76:132-6.

7. Miguez PA, Castro PS, Nunes MF, Walter R, Pereira PN. Effect of acid-etching on the enamel bond of two self-etching systems. J Adhes Dent 2003;5:107-12.

8. Perdigão J, Geraldeli S. Bonding characteristics of self-etching adhesives to intact versus prepared enamel. J Esthet Restor Dent 2003;15:32-41.

9. Rotta M, Bresciani P, Moura SK, Grande RH, Hilgert LA, Baratieri LN, et al. Effects of phosphoric acid pretreatment and substitution of bonding resin on bonding effectiveness of self etching systems to enamel. J Adhes Dent 2007;9:537-46.

10. Nasr K, Sharrock P, Grégoire G. Release of aqueous calcium and phosphate from human dental enamel following administration of self-etching adhesives. J Biomater Sci Polym Ed 2005;16:745-59.

11. Senawongse P, Sattabanasuk V, Shimada Y, Otsuki M, Tagami J. Bond strength of current adhesives systems on intact and ground enamel. J Esthet Restor Dent 2004;16:107-15.

How to cite this article: Devarasa GM, Subba Reddy VV, Chaitra NL. Self etching adhesive on intact enamel. J Indian Soc Pedod Prev Dent 2012;30:133-8.

Source of Support: Nil, Conflict of Interest: None declared.

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