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 Table of Contents  
Year : 2023  |  Volume : 15  |  Issue : 1  |  Page : 14-20

Investigation of shear bond strength of different adhesive agents to demineralized enamel with or without resin ınfiltration

1 Department of Restorative Dentistry, Health Sciences University, Istanbul, Turkey
2 Department of Restorative Dentistry, Ataturk University, Erzurum, Turkey
3 Department of Restorative Dentistry, Pamukkale University, Denizli, Turkey

Date of Submission23-Nov-2021
Date of Decision05-Apr-2022
Date of Acceptance08-Apr-2022
Date of Web Publication29-Dec-2022

Correspondence Address:
Merve Iscan Yapar
Department of Restorative Dentistry, Faculty of Dentistry, Ataturk University, Erzurum - 25240
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Source of Support: None, Conflict of Interest: None

DOI: 10.4103/jorr.jorr_78_21

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Objectives: This study aimed to investigate the bond strength of adhesive agents to enamel surfaces with and without resin infiltration.
Materials and Methods: The crowns and roots of 198 human incisors were separated from each other and placed in an acrylic mold. The teeth were ground until the guide grooves created with the slotted bur disappeared. Then, it was thrown into the demineralization solution and artificial caries lesions were created. Teeth were randomly divided into two main groups, and each main group was divided into five subgroups. And also the control group was determined. The materials and composite were applied to demineralized enamel. For the shear bond analysis, a universal testing machine was used. Statistical analysis of the data was evaluated by one-way ANOVA test and independent t-test.
Results: The result showed that there was no statistical difference between no resin infiltrant adhesive bonding agent groups (P < 0.05) and no difference between resin-treated groups and untreated groups of each bonding agent (P < 0.05). Furthermore, there is no difference between resin infiltrant pretreated adhesive bonding agent groups (P < 0.05).
Conclusion: The use of different adhesive systems during restorative procedures after resin infiltration did not affect the shear bond strength.

Keywords: Dental adhesive agent, resin infiltration, self-etch adhesive, shear bond strength, universal bonding

How to cite this article:
Bilgic R, Yapar MI, Celik N, Akgul N. Investigation of shear bond strength of different adhesive agents to demineralized enamel with or without resin ınfiltration. J Oral Res Rev 2023;15:14-20

How to cite this URL:
Bilgic R, Yapar MI, Celik N, Akgul N. Investigation of shear bond strength of different adhesive agents to demineralized enamel with or without resin ınfiltration. J Oral Res Rev [serial online] 2023 [cited 2023 May 30];15:14-20. Available from: https://www.jorr.org/text.asp?2023/15/1/14/365925

  Introduction Top

Large active white spot lesions may contain cavitating lesions that require restorative treatment and superficial lesions.[1] In such lesions, the use of infiltrant for areas showing demineralization and a bonding agent for advanced lesions will ensure that the procedure is easy and in a short time. The resin infiltrant to be used for this purpose should be able to be bonded to enamel at least as much as a conventional adhesive.[2] The resin infiltration technique is a new technology for healing early enamel caries (Icon, DMG, Hamburg, Germany). This technique is a minimally invasive approach that can be applied instead of traditional methods that will cause the loss of healthy tooth hard tissue in initial enamel caries without cavitation.[3] This method is a new treatment option among preventive and restorative applications and aims to penetrate the deep of the lesion.[4] Resin infiltration can be used to stop the lesions in a single session without the need for anesthesia and the use of drills.[3] In recent studies, it has been observed that the application of resin infiltrant decreases the rate of lesion progression.[5] It also infiltrates the micropores of the lesion and masks the appearance of the white spot lesion.[6]

There are three different strategies in dental adhesion technology: etch and rinse and self-etch bonding systems and universal bonding systems. It is recommended to use acetone-based etch and rinse systems by the “wet bonding” technique.[7] However, in practice, it is not possible to dry the enamel while leaving the dentin moist and to determine whether the dentin is wet or dry enough.[8] The problem of dentin moistness, which reduces the spreading of the adhesive resin between collagen fibers, has been eliminated with self-etch adhesive systems. However, the acids in self-etch adhesives are weak to phosphoric acid and resulting in lower binding to the enamel.[9] To prevent this situation, it is recommended to selectively etch only the enamel edges of the cavity before the application of self-etch adhesives. In practice, however, dentin may also be exposed to acid during enamel etching. Recently, various studies have been conducted to eliminate the disadvantages of single-stage self-etch adhesives that provide ease of use clinically, and as a result, “universal” or “multimode” products have been created.[10] These products can be used as self-etch, selective etching, and etch and rinse.

The aim of this study is to investigate the effect of different bonding agents on the shear bond strength (SBS) of demineralized enamel with and without resin infiltrant. The null hypothesis tested in this study was that the SBS of the resin infiltrant system on demineralized enamel is not significantly different from adhesives tested, and pretreatment with the resin infiltrant does not impair the SBS of the different from adhesives.

  Materials and Methods Top

In this study, 198 human upper central incisors, which were removed for periodontal reasons in the past 6 months, without caries and defects in the crown part, were used. The attachments on the teeth were removed and the teeth were kept in refreshed distilled water every week during the experiment. Tooth specimens were measured with a laser fluorescence device (DIAGNOdent PEN®, KaVo, Zurich), and teeth with good scores (0–13) were included in the study.

The crowns and roots of the teeth were removed from the enamel-cement border by cutting with a low-speed cutting device (IsoMet® Low-Speed Saw, Buehler®, Illinois, USA) under water cooling. Teeth were embedded in transparent acrylic so that the vestibule surfaces remain outside. First, 0.5-mm deep grooves were created on the facial surface of the teeth with depth-determining burs. The deepest groove was marked with a pencil. The samples were sanded to the point where these marks on the tooth surface first disappeared using 320, 600, and 1200 grit aluminum oxide (Al2O3) abrasive paper discs. In our study, the demineralization solution used to create an initial enamel lesion on the teeth was prepared in the Department of Clinical Biochemistry at Atatürk University Faculty of Medicine, as suggested by Yang et al.[11]

Demineralization solution

0.075 mol 1–1 glacial acetic acid, 0.002 mol 1–1 Ca (from CaCl2), and 0.002 mol of 1–1 P (from KH2PO4) were created and its pH was adjusted to 4.6. To create initial enamel caries, tooth samples were kept in the demineralization solution at 37°C until scores between 14 and 20 with DIAGNOdent PEN® were obtained.

Demineralized teeth were divided into two main groups and then these main groups were divided into five subgroups. One group was determined as the control group. In total, 11 groups were formed with 18 teeth in each group. Group 1: Icon (control group). Only Icon resin infiltration material was applied to the samples in this group. First, 15% hydrochloric acid gel was applied to the demineralized enamel surface for 2 min. Then, the acid was removed using water spray for 30 s. With the hydrochloric acid, the hypermineralized layer that would prevent the penetration of the resin was removed. Ninety-nine percent ethanol (Icon Dry, DMG) was applied for 30 s to remove the water in the microporosity in the demineralization area and air-dried. After this procedure, the white appearance of the demineralized areas became more pronounced. Afterward, resin infiltrant (Icon Infiltrant; DMG) was applied to the demineralized surface with the help of a micro brush for 3 min in the first application and 1 min in the second application. After each application, it was polymerized with a light device (Woodpecker LED Polymerization Device) for 40 s.

Group 2: Icon + Clearfil SE Bond (Kuraray Medical, Okayama, Japan). In addition to applying the ICON resin infiltrant, the primer of Clearfil SE Bond was applied for 20 s according to the user instructions and air-dried. Afterward, the Clearfil SE Bond adhesive agent was applied in a thin layer. It was dried with a light air spray and light-cured for 10 s.

Group 3: Icon + Clearfil S3 Bond (Kuraray Medical INC.1621 Sakazu, Kurashiki, Okayama 710–0801, Japan). In addition to the ICON resin infiltrant application, Clearfil S3 Bond was applied to the demineralized enamel surface with the help of the applicator according to the user instructions. After waiting for 20 s, it was spread on the surface with light air and polymerized for 10 s.

Group 4: Icon + Adper Single Bond 2 (3M ESPE St. Paul, MN, USA). In addition to the ICON resin infiltrant application, acid was applied to the demineralized enamel surface for 30 s. It was thoroughly washed with water and dried. Two coats of Adper Single Bond were applied, lightly air was squeezed, and the bond was spread into the cavity. Then, it was polymerized for 10 s.

Group 5: Icon + Single Bond Universal (3M ESPE St. Paul, MN, USA). In addition to the application of ICON resin infiltrant, Single Bond Universal adhesive was applied to the demineralized enamel surface. It was air-dried and light-cured for 10 s.

Group 6: Icon + Scotchbond acid + Single Bond Universal. In addition to the ICON resin infiltrant application, Scotchbond acid was applied to the demineralized enamel surface for 30 s according to the user instructions and then washed. Single Bond Universal adhesive was applied. It was air-dried for 5 s and light-cured for 10 s.

Group 7: SE Bond. Primer of Clearfil SE Bond was applied for 20 s and lightly air-dried according to user instructions. Afterward, the Clearfil SE Bond adhesive was applied in a thin layer. It was dried with a light air spray and light-cured for 10 s.

Group 8: S3 Bond. Clearfil S3 Bond was applied to the demineralized enamel surface with the help of an applicator. After waiting for 20 s, it was spread on the surface with light air and polymerized with a light device for 10 s.

Group 9: Adper Single Bond 2. Acid was applied to the demineralized enamel surface for 30 s, washed with plenty of water, and dried. Two layers of Adper Single Bond were applied and the bond was spread into the cavity with light air. Afterward, it was polymerized with a light device for 10 s.

Group 10: Single Bond Universal. Single Bond Universal adhesive was applied to the demineralized enamel surface. It was air-dried for 5 s and light-cured for 10 s.

Group 11: Scotchbond acid + Single Bond Universal. Scotchbond acid was applied to the demineralized enamel surface for 30 s and then washed with air-water spray. Single Bond Universal Adhesive was applied. It was air-dried for 5 s and light-cured for 10 s.

The contents of the materials used in the study are shown in [Table 1]. The materials were applied on demineralized enamel according to the manufacturer's recommendations. Cylindrical transparent molds with an inner diameter of 3 mm and a height of 4 mm were prepared for the standard application of composite resin (Clearfil Majesty Esthetic, Kuraray Medical, Okayama, Japan) to the prepared tooth samples, and composite resin was applied in two 1.5 mm layers and cured with light for 60 s. All specimens were kept in distilled water at 37°C for 24 h and were subjected to SBS testing with a universal testing machine (Instron 3344, Instron Corp., Wilmington, USA). This machine included a special blade applied to the adhesive interface at a crosshead speed of 1 mm/min. Specimens were exposed to stress until failure occurred, and the load per area was expressed in megapascals (MPa). Data were analyzed using one-way ANOVA and Tukey's post hoc test to compare the SBS values. Independent-samples t-test was used to compare the SBS values of the adhesive groups with and without resin infiltration. The level of significance was set at P < 0.05.
Table 1: Materials used in the present study

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  Results Top

The SBS values of the adhesive bonding materials applied on the demineralized enamel surface according to the resin-infiltrated and nonresin-infiltrated groups are shown in [Table 2]. When the SBS between the groups without resin infiltration was compared, no statistically significant difference was found between the adhesives (P < 0.05). When the resin-infiltrated groups were compared, there was no statistically significant difference between the adhesives (P < 0.05).
Table 2: Statistical analysis of ANOVA

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[Table 3] shows the results of the SBS tests according to groups with and without resin infiltration technique. The minimum mean value of SBS was 989 MPa for Group 8 [Table 3a], and the maximum mean value was 16.6 MPa for Group 11 [Table 3b]. Overall, all experimental adhesive systems exhibited lower mean values of SBS compared with that of the universal adhesive with acid etching. ANOVA revealed that the SBS value of universal adhesives without resin infiltration was significantly higher than that of the other groups (P < 0.05). Resin infiltration with no adhesives (Icon control group) showed significantly lower SBS than universal adhesives with acid etching (P < 0.05), and there were no significant differences in the SBS values among the other adhesive groups (P > 0.05). When the SBS of the adhesive groups with and without resin infiltration was evaluated, it was observed that the differences between the groups were not statistically significant (P < 0.05) [Table 4].

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Table 4: Independent t-test results

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The enamel specimen surfaces were examined under a stereomicroscope (SZ-PT Olympus, Japan). Failure types were classified based on the amount of resin composite remaining on the enamel surface (<20% adhesive failure, 20%–80% mixed failure, and >80% cohesive failure). Failure types are shown in [Table 5]. According to the failure mode analysis results, the dominant failure mode was adhesive failure (43.4%), followed by cohesion failure (38.3%). Mixed failure was least failure type for all groups (18.1%).
Table 5: Failure types of the experimental groups after shear bond strength testing

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Adhesive breakage was more common in the control group (8%–44.4%), Group 2 (8%–44.4%), Group 4 (9%–50%), and Group 5 (8%–44.4%); cohesive type fracture was more common in Group 3 (8%–44.4%) and Group 6 (8–44.4%).

While adhesive type fracture was dominant in Group 7 (8%–44.4%), Group 8 (8%–44.4%), Group 10 (8%–44.4%), and Group 11 (8%–44.4%), cohesive type fracture was more common in Group 9 (9%–50%).

  Discussion Top

This in vitro study demonstrated that the adhesive performance of the resin infiltrant was similar to other bonding agents and that adhesive bonding did not impair the bond strength of teeth pretreated with resin infiltrant. Therefore, the null hypothesis was accepted.

It has been observed that different tooth groups are used for the example of studies on the treatment of initial caries. The more commonly used these are human teeth and bovine teeth.[2] It is known that the enamel of veal teeth is affected more by the demineralization solution applied than human enamel. In addition, due to this porous structure, the surface structure changes more during the experiments.[12] Therefore, in our study, periodontally extracted human upper central teeth without carious lesions were used.

Artificial caries lesions created in an in vitro environment do not have the same characteristics as natural caries lesions developing in the oral environment.

However, artificial lesions are frequently used in studies because they have similar properties to natural lesions.[13] In this study, the initial caries lesion was obtained by keeping the samples in containers with a demineralization solution with the same amount and content and pH for 48 h with an acetic acid-based solution.[11]

In an in vitro study by Shi et al., DIAGNOdent measurements were compared with radiographic and histopathological examinations in the detection of demineralization areas formed on flat surfaces, and it was determined that DIAGNOdent was effective in identifying flat surface caries lesions.[14] In the study of Reis et al. comparing the performance of DIAGNOdent in vivo and in vitro conditions, it was reported that the accuracy rate in vitro conditions was higher.[15] In the light of these studies, the DIAGNOdent PEN device was used to diagnose and standardize artificial caries lesions in our study.

In the literature reviews, it has been observed that there is no study comparing the bonding strength of resin infiltrant application and adhesive bonding agents, especially universal bonding systems. For these reasons, we think that our study will add new information to the literature. SBS tests are one of the frequently preferred methods for evaluating dental materials and techniques under in vitro conditions.[16] In this study, the SBS test was preferred because it is a practical and common method.

Researchers still consider three-stage etch and rinse adhesives the “gold standard” for bond strength. It is claimed that the closest values to this adhesive are only for two-step self-etch adhesives.[17],[18] Two-stage self-etch, one-stage self-etch, and two-stage total-etch and universal bonding agents were included in our study to compare resin infiltrant and adhesive systems. There are contradictions in studies comparing self-etch, etch and rinse systems, and universal adhesives in the literature. Mueller et al. reported that the acidic monomers of self-etch adhesives were not sufficient to remove the surface layer and could not create a good penetration compared to total-etch systems.[4] Perdigão et al.[19] reported that Single Bond Universal adhesive provided better bonding to dentin tissue than Clearfil SE Bond, while Muñoz et al.[20] reported that they obtained higher bonding values in the group using Clearfil SE Bond in their study comparing universal bonding agents and self-etch adhesives. Suzuki et al. reported that two-step self-etch systems were more successful in their study comparing the SBS of two-step self-etch adhesives with universal adhesives.[21] Suzuki et al., in their study comparing various universal bonding agents in total-etch and self-etch mode, found the bond strength in the total-etch mode to be statistically higher than in the self-etch mode.[22] In our study, when the groups without resin infiltration were compared among themselves, the acid + universal bonding group (Group 11) was found to be statistically higher than the others. Although there was a numerical difference between the other groups, there was no statistical difference. Total etch bonding systems show better bond strength than self-etch bonding agents.[17] Therefore, in our study, the universal bond showed a higher value in total-etch mode than in self-etch mode. The reason for the statistical difference in our study may be the application of acid to the enamel as a pretreatment. In this way, the bonding agent may have penetrated deeper into the enamel surface. The superiority of the acid + universal bond group over the Single Bond 2 group, which is total-etch bonding, can be explained by the chemical bonding potential of functional adhesive monomers such as 10-methacryloyloxydecyl dihydrogen phosphate (MDP) monomers with hydroxyapatite calcium in the universal bonding agent.[23] This MDP monomer forms a superficial demineralization and a more stable salt complex on the tooth surface.[24] These salt bridges also contribute to the protection of the hybrid layer. Thus, it may have shown a better bond strength. It is thought that the superficial formation of artificial lesions and the deep penetration depth of the adhesive are effective in the close bond strength values.

Jia et al. investigated the effect of resin infiltrant application on the bond strength of different adhesives in demineralized and intact enamel. As a result, they reported that the bond strength of resin infiltrant and total-etch systems was similar and that resin infiltrant material in demineralized enamel did not impair or even increase the bond strength of self-etch and total-etch adhesives.[25] Similar to this study, in our study, a statistical difference was not found between the resin infiltrant applied samples and the total-etch systems in terms of bond strength. In another in vitro study by Naidu et al., it has been stated that using Icon® before attaching brackets to demineralized enamel does not reduce the SBS of orthodontic resin cement; on the contrary, it increases the SBS of the orthodontic resin cement, and also reduces the fractures that may occur in the enamel during the removal of the brackets.[26] It was stated that the application of resin infiltrant on the enamel surface before orthodontic treatment increased the SBS of the bonding agent used in the in vitro study by Mews et al.[27] Contrary to the results of these studies, there was no statistically significant difference between the resin-infiltrated and nonresin-infiltrated groups in the present study. The resin infiltration material did not increase the binding of the adhesive agents. The reason for this is thought to be that the properties of the resin material are effective. The high content of triethylene glycol dimethacrylate (TEGDMA) reduces the viscosity of the resin infiltrant and the contact angle with the enamel, increasing its penetration ability.[28] On the other hand, the increase in the TEGDMA ratio causes the polymerization shrinkage of the resin and the polymerization stress to increase.[29] In addition, an inhomogeneous resin layer is formed due to the formation of an oxygen inhibition zone on the surface or insufficient evaporation of the solvent.[30]

Although it is thought that the resin infiltrant material will create more bonding strength than other adhesive agents due to the TEGDMA content, the low molecular weight and the hydrophilic hydroxyethyl methacrylate monomer of traditional adhesive agents provide an effective adhesion and a high bond strength. Another reason that increases the bonding strength of dental adhesive agents is that the initial enamel lesion created is more superficial than natural carious lesions. In this way, the adhesives can infiltrate the enamel completely and the bond strength can be increased. Due to all these properties, the resin infiltrant material may not have increased the bond strength of the adhesive agents. It was reported that the SBS of Icon® applied to the artificially created initial enamel lesion was 17.5 MPa, and the bond strength of the adhesive material (Heliobond, Ivoclar Vivadent, Liechtenstein) was 15 MPa in an in vitro study by Wiegand et al.[2]

The reason that there was no statistical difference between the control group treated with Icon and other dental adhesives is thought to be due to the high TEGDMA and hydrochloric acid content of Icon resin material, and thus, it is thought that better penetration depth and bond strength are formed. In addition, for TEGDMA to penetrate deep into the demineralized area of the enamel, the pores of the lesion must be clean and dry. Ninety-nine percent ethanol (Icon Dry) in the resin infiltration application ensures the removal of excess water from the pores and increases the deeper penetration of TEGDMA, a “hydrophilic” and low-viscosity monomer[31] on the enamel surface. Due to this feature, the bond strength of the control group may have shown a similar value to the adhesive groups.[32]

In SBS studies, it is reported that the most common type of fracture in enamel-composite interfaces is “adhesive” type fractures.[33] In our study, generally adhesive and cohesive type breakages were observed equally. These results can be explained by the cohesion breaking on the surface due to demineralized enamel, which is more likely to break under stress. It can also be explained by the adhesive breakage due to the higher cohesion strength of the composite used.

  Conclusion Top

According to the findings, since there are no statistically significant differences when comparing different dental adhesive agents and resin infiltration material in terms of bond strength, the composite material can be applied without using a bonding agent again, if appropriate isolation conditions are observed in teeth with initial carious lesions with resin infiltration. Furthermore, when considering using a bonding agent, any etch and rinse, self-etch, and universal adhesive agents can be chosen. We think that conducting more in vitro and in vivo studies on this subject will contribute to obtaining more accurate results.

Ethical clearance

Since this study was an in vitro study, the ethics committee report was not received.


Our work was not supported by any institutional or educational funding source. This study was presented as an oral presentation at the Esthetic Dentistry Association 21st International Congress of Esthetic Dentistry.

Financial support and sponsorship


Conflicts of interest

There are no conflicts of interest.

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Kielbassa AM, Muller J, Gernhardt CR. Closing the gap between oral hygiene and minimally invasive dentistry: A review on the resin infiltration technique of incipient (proximal) enamel lesions. Quintessence Int 2009;40:663-81.  Back to cited text no. 3
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  [Table 1], [Table 2], [Table 3], [Table 4], [Table 5]


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