TMP CE5 C
TMP CE5 C
TMP CE5 C
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PURPOSE. This study evaluated the adhesion of 10-MDP containing self-etch and self-adhesive resin cements to
dentin with and without the use of etch-and-rinse technique. MATERIALS AND METHODS. Human third molars
(N=180) were randomly divided into 6 groups (n=30 per group). Conventional (Panavia F2.0, Kuraray-PAN) and
self-adhesive resin cements (Clearfil SA, Kuraray-CSA) were bonded to dentin surfaces either after application of
3-step etch-and-rinse (35% H3PO4 + ED Primer) or two-step self-etch adhesive resin (Clearfil SE Bond).
Specimens were subjected to shear bond strength test using the universal testing machine (0.5 mm/min). The
failure types were analyzed using a stereomicroscope and quality of hybrid layer was observed under a scanning
electron microscope. The data (MPa) were analyzed using two-way ANOVA and Tukey’s tests (α=.05). RESULTS.
Overall, PAN adhesive cement showed significantly higher mean bond strength (12.5 ± 2.3 - 14.1 ± 2.4 MPa)
than CSA cement (9.3 ± 1.4 - 13.9 ± 1.9 MPa) (P<.001). Adhesive failures were more frequent in CSA cement
groups when used in conjunction with two-step self-adhesive (68%) or no adhesive at all (66%). Hybrid layer
quality was inferior in CSA compared to PAN cement in all conditions. CONCLUSION. In clinical situations
where bonding to dentin substrate is crucial, both conventional and self-adhesive resin cements based on
10-MDP can benefit from etch-and-rinse technique to achieve better quality of adhesion in the early clinical
period. [ J Adv Prosthodont 2013;5:226-33]
KEY WORDS: Adhesion; Bond strength; Dentin; Hybrid layer; Self-adhesive cement
INTRODUCTION chanical retention between the resin cement and the dentin
tubuli takes place when the adhesive resin penetrates into
The adhesion mechanism of resin cements to dental tissues the intratubular and intertubular dentin, forming resin tags
and especially to dentin, has been studied thoroughly in the and the hybrid layer.1 Micromechanical interlocking is the
last few decades. The establishment of effective microme- most important adhesion mechanism of resin to dentin.
However, several factors such as acid-etching, moisture
condition of the tooth, penetration depth of adhesive resin
Corresponding author: into dentin and dentin depth can affect the formation of
Volkan Turp
Department of Prosthodontics, Faculty of Dentistry, University of Istanbul, hybrid layer and resin tags.2
34093 Fatih Istanbul, Turkey The dentin bonding mechanism is essentially based on
Tel. 905353521632: e-mail, [email protected]
Received December 6, 2012 / Last Revision July 16, 2013 / Accepted the infiltration of resin monomers into the porosities creat-
August 7, 2013 ed by removal of mineral or inorganic material from the
© 2013 The Korean Academy of Prosthodontics dental tissues. This exchange results in micro-mechanical
This is an Open Access article distributed under the terms of the Creative interlocking in the porosities formed.3,4 Successful dentin
Commons Attribution Non-Commercial License (http://creativecommons.
org/licenses/by-nc/3.0) which permits unrestricted non-commercial use, bonding could be achieved through several routes. The so-
distribution, and reproduction in any medium, provided the original
work is properly cited.
called “etch-and-rinse” technique is the conventional three-
step adhesion procedure. The tooth substrate is first etched
226
Adhesion of 10-MDP containing resin cements to dentin with and without the etch-and-rinse technique
with 30-40% phosphoric acid (H3PO4) and then rinsed off. of 2.0 mm thickness from the occlusal surfaces of the teeth
Following acid etching, adhesive resin is applied on the were removed by means of a slow-speed diamond saw
conditioned tooth surface. For dentin, the bonding mecha- (Isomet, Buehler Ltd. Lake Bluff, IL, USA) under water-
nism of etch-and-rinse adhesives primarily depends on cooling to expose flat deep dentin surfaces. Standardization
micro-mechanical retention of resin with the exposed colla- of smear layer was achieved by grinding the dentin surfaces
gen fibrils. For enamel, total etch technique is the most with 600 grit silicon carbide paper.
effective and reliable method for long-term clinical success.5 The adhesive systems were applied according to the
In the “self-etch” approach, adhesives condition and manufacturers’ instructions. Application procedures and
prime dentin are applied at the same time, and no rinsing is product information is displayed in Table 1. A transparent
required. In this procedure the clinical application time is polyethylene mold (diameter: 4 mm and height: 6 mm) was
shortened and technique sensitivity is significantly reduced. used to bond the resin cements onto dentin surfaces (Fig.
Self-etch adhesives can be categorized as “mild” and 1A).
“strong”. Strong self-etch adhesives with functional mono- In Group 1, conventional adhesive resin cement
mers have low pH (<1) and their bonding mechanism is (Panavia F 2.0, Kuraray, Tokyo, Japan) (PAN) was applied
reported to be similar to etch-and-rinse adhesives. ‘Mild’ following etch-and-rinse and bonding (ED Primer,
self-etch adhesives (pH≈2) selectively demineralize the den- Kuraray). In Group 2, PAN resin cement was applied fol-
tin surface and are reported to form a shallow hybrid layer. lowing bonding (ED Primer) without acid etching. In
Adhesion is ensured by chemical interaction between resid- Group 3, self-adhesive resin cement (Clearfil SA, Kuraray)
ual hydroxyapatite and functional monomers.6 (CSA) was applied following etch-and-rinse and bonding
Several self-etching adhesive systems contain specific (Clearfil SE, Kuraray). In Group 4, CSA resin cement was
functional monomers which enhance the performance of applied following bonding (Clearfil SE) without acid etch-
adhesion. The functional monomers may help conditioning ing. In Group 5, only CSA resin cement was applied onto
dental tissues, increase monomer penetration, 7 and also dentin surfaces neither with acid etching nor bonding.
improve the chemical adhesion to hard tissues of the Lastly, in Group 6, only PAN resin cement was applied
tooth.8 10-methacryloyloxydecyl dihydrogen phosphate (10- onto dentin surfaces neither with acid etching nor bonding.
MDP) is one of the most commonly used functional Light activation was performed for 20 seconds, using a
monomers;9 it is the hydrophilic phosphate monomer that quar tz tungsten halogen curing device (Hilux 200,
increases resin diffusion and adhesion by causing acidic Benlioglu, Ankara Turkey) with irradiance of 600 mW/cm2.
decalcification and binding to calcium ions or amino The specimens were stored for 24 hours in dark at room
groups of tooth structure.10 It is reported to be one of the temperature prior to bond strength tests.
most successful materials in the market for chemical bond-
ing.11,12 On the other hand, self-adhesive cements do not Bonding strength was evaluated using a mechanical
require conditioning the dentin or ceramic surfaces. Such shear test. Specimens were placed firmly in the universal
cements have multifunctional phosphoric acid dimethacry- testing machine (Shimadzu AG-IS, Shimadzu, Kyoto, Japan)
late modified monomers.2 However, their diffusion level and the shear force was applied until fracture of the speci-
into dentin and their hydrolytic stability are not optimal.12-17 men (Fig. 1B). The load was applied at the dentin/adhesive
Adhesion to deeper tooth substrates with contemporary interface, as close to the surface of the tooth as possible. A
strong adhesives is an interesting subject which is not stud- crosshead speed of 0.5 mm/min was used for loading.
ied thoroughly in the literature. The objectives of this study Subsequently, specimens were evaluated under optical
were to evaluate the adhesion of two different 10-MDP microscope (Leica M80, Leica Microsystems, Wetzlar,
containing adhesive resin cements to deep dentin using Germany) at ×40 magnification in order to investigate the
either etch-and-rinse or two-step self-etch bonding tech- mode of failure. The types of failures were categorized as;
niques and analyze the failure types. The null hypothesis adhesive failure between tooth and resin cement (A), cohe-
tested was that adhesion of 10-MDP containing resin sive failure of resin cement (C) or mixed failure where resin
cements would not show difference when used in combina- cement was failed partially cohesively and partially adhe-
tion with etch-and-rinse or two-step self-etch system. sively on the specimen (M).
MATERIALS AND METHODS The specimens were sectioned longitudinally and inter-
faces were wet polished with silicone carbide papers of
This study was approved by the Ethics Research Committee #600, #1000, #1200 grit in sequence. Following polishing,
of Istanbul University Faculty of Medicine (Istanbul the interfaces were decalcified (37% H3PO4 for 10 seconds)
University, Istanbul, Turkey) (Approval no: 2013/317). and deproteinized (2% NaOCl solution for 1 minute) in
Intact human third molars without caries (N=180) were order to evaluate the hybrid layer.
used for this study. The roots of the teeth were embedded The hybrid layer and surface pattern were investigated
in auto-polymerized acrylic resin (Takilon, SPD Salmoiraghi for all experimental groups using scanning electron micros-
Produzione Dentaria S.r.l Mulazzano, Italy) and randomly copy (SEM) (JSM 7000F, JEOL, Japan) by selecting one
divided into 6 groups (n=30 per group). Dental materials specimen with bonding strength closest to mean value of
Table 1. Brands, manufacturers, chemical compositions and application protocols of the materials used in the study
Manufacturer
Material Composition Application
(Lot No.)
A B
Fig. 1. (A) schematic diagram of specimen and (B) the shear testing.
228
Adhesion of 10-MDP containing resin cements to dentin with and without the etch-and-rinse technique
the group. The specimens were covered with a thin layer of did not significantly increase the bond strength of CSA
platinum (Sputter-coated) for SEM observation. The whole cement when compared to direct application (9.3 ± 1.4
fractured surface at the dentin side was observed under the MPa) (P>.05). Similarly, for the PAN adhesive cement the
SEM. bond strength did not differ significantly between bond-
ing(12.5 ± 2.3 MPa) and direct applications (12.8 ± 2.6
Statistical analysis was performed using SPSS 11.0 soft- MPa) (P>.05).
ware for Windows (SPSS Inc., Chicago, IL, USA). The Adhesive failures were more frequent in CSA cement
assumptions of normality and equal variances across groups when used in conjunction with two-step self-adhe-
groups were validated. Bond strength data (MPa) were sub- sive (68%) or no adhesive at all (66%) compared to other
mitted to analysis of variance (two-way ANOVA). Multiple groups (37-43%) (Table 3). Generally, specimens with lower
comparisons were made with Tukey's post-hoc test (α=.05) bond strengths failed to bond adhesively.
with the shear bond strength as the dependent and adhe- SEM observations demonstrated well-defined hybrid
sion protocols and the cement types as the independent layer with visible resin tags in dentin in PAN cement group
factors. P values less than .05 were considered to be statisti- on 35% H 3 PO 4 conditioned dentin and ver y minor
cally significant in all tests. detached areas were also evident at the interface (Fig. 2).
The unconditioned dentin specimens presented thinner
RESULTS hybrid layer and less frequent distribution of resin tags (Fig.
3).
Overall, PAN adhesive cement showed significantly higher Hybrid layer quality was inferior in CSA compared to
mean bond strength (12.5 ± 2.3 - 14.1 ± 2.4 MPa) than PAN cement in all conditions. On CSA specimens, resin
CSA cement (9.3 ± 1.4 - 13.9 ± 1.9 MPa) (P<.001) (Table tags were also visible on both H 3PO 4 conditioned and
2). Etching dentin with 35% H 3 PO 4 increased bond unconditioned dentin surfaces (Fig. 4, Fig. 5 and Fig. 6).
strength significantly for both PAN (14.1 ± 2.4 MPa) and Although resin tag formation was present, resin cement
CSA (13.8 ± 1.9 MPa) compared to the application of two- showed detached areas from dentin (Fig. 4). On uncondi-
step self-etch adhesive resin (12.5 ± 2.3 - 9.8 ± 1.6 MPa, tioned dentin surfaces a superficial interaction and a thin
respectively) (P<.05). hybrid layer formation was apparent compared to PAN
Application of bonding agent on dentin (9.8 ± 1.6 MPa) (Fig. 7).
Table 2. Mean shear bond strengths (MPa) for each group. Results of the post-hoc tests are
indicated by superscripted letters. Groups labelled with different superscripted letters are
significantly different (P<.05)
Table 3. Percentage distribution of failure modes per group (A: Adhesive, C: Cohesive, M:
Mixed)
Group A C M
Fig. 2. SEM micrograph of cement-dentin interface luted Fig. 3. SEM micrograph of cement-dentin interface luted
with Panavia F2.0 and bonded on etched and rinsed with Panavia F2.0 and bonding on unconditioned dentin,
dentin, where a thick hybrid layer (1) and uniform where hybrid layer is thinner compared to acid
distribution of resin tags (2) are visible observed. (Group conditioned group of the same material (1). Also resin
1) (×1,000 magnification). tags are weak (2) and are not infused into dentin tubules
homogenously (3) (Group 2) (×1,000 magnification).
Fig. 4. SEM micrograph of cement-dentin interface luted Fig. 5. SEM micrograph of cement-dentin interface luted
with Clearfil SA cement and bonding on etched and with Clearfil SA cement bonded on unconditioned
rinsed dentin, where irregular hybrid layer (1) and resin dentin, where hybrid layer is very thin and not present in
tag formations (2) are observed (Group 3) (×1,000 some areas (1), resin tags are very few (2) and dentin
magnification). tubules are mostly empty (3) (Group 4) (×1000
magnification).
230
Adhesion of 10-MDP containing resin cements to dentin with and without the etch-and-rinse technique
Fig. 6. SEM micrograph of cement-dentin interface luted Fig. 7. SEM micrograph of cement-dentin interface luted
with Clearfil SA cement on unconditioned dentin, where with Panavia F2.0 cement on unconditioned dentin,
hybrid layer is almost not present (1) and number of resin adhesive failure can be observed (Group 6) (×1000
tags are very few in number (2) with empty dentin magnification).
tubules (3) (Group 5) (×1000 magnification).
SEM micrographs of PAN cement applied dentin displayed consider this especially in situations where adhesion is tak-
a thicker and attached hybrid layer on etched and rinsed ing place mostly to dentin tissues, such as large inlay or
dentin. On the other hand, CSA cement applied dentin onlay restorations and excessively prepared teeth for fixed
showed thinner hybrid layer and detached local areas. Other dental prostheses.
reasons for this could be the variations in mechanical prop-
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