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journal of dentistry 37 (2009) 769775

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Improving the effect of NaOCl pretreatment on bonding


to caries-affected dentin using self-etch adhesives
Gen Taniguchi a,*, Masatoshi Nakajima a, Keiichi Hosaka a, Nanako Iwamoto a,
Masaomi Ikeda b, Richard M. Foxton c, Junji Tagami a,d
a

Cariology and Operative Dentistry, Department of Restorative Science, Graduate School, Tokyo Medical and Dental University,
1-5-45 Yushima, Bunkyo-ku, Tokyo 113-8549, Japan
b
Faculty of Dentistry, School for Dental Technology, Tokyo Medical and Dental University, 1-5-45 Yushima, Bunkyo-ku, Tokyo 113-8549, Japan
c
Department of Conservative Dentistry, Kings College London Dental Institute at Guys, Kings College and St. Thomas Hospitals,
Kings College London, London Bridge, London SE1-9RT, UK
d
Global Center of Excellence (GCOE) Program, International Research Center for Molecular Science in Tooth and Bone Diseases at Tokyo
Medical and Dental University, 1-5-45 Yushima, Bunkyo-ku, Tokyo 113-8549, Japan

article info

abstract

Article history:

Objective: To evaluate the effect of sodium hypochlorite pretreatment on adhesion to

Received 28 January 2009

normal and caries-affected dentin using self-etch adhesives.

Received in revised form

Methods: Forty extracted human molars with coronal carious lesions were used in this

9 May 2009

experiment. The occlusal dentin surfaces including the caries-affected dentin in each group

Accepted 2 June 2009

were treated as follows: group 1, rinsed with water; group 2, treated with 6% NaOCl for 15 s;
group 3, treated with 6% NaOCl for 30 s; group 4, application with Accel for 30 s after NaOCl30 s pretreatment. After rinsing with water and air-drying, the treated dentin surfaces were

Keywords:

applied with self-etch systems (Bond Force and Clearfil Protect Bond) according to the

Smear layer

manufacturers instructions, and built-up with resin composite. After 37 8C water storage

Caries-affected dentin

for 24 h, the bonded normal or caries-affected dentin areas were isolated to create an

Dentin bonding

hourglass configuration with a cross-sectional area of approximately 1 mm2. The specimens

NaOCl

were subjected to tensile stress at a cross-head speed of 1.0 mm/min.

Antioxidant

Results: NaOCl-15 s pretreatment significantly improved the mTBS of both self-etch adhesives to caries-affected dentin, while the 30 s pretreatment did not affect them. For normal
dentin, NaOCl-30 s pretreatment significantly reduced the mTBS of both self-etch adhesives
although the 15 s pretreatment did not alter them. Furthermore, the application of Accel
with a reducing effect increased the mTBS to normal and caries-affected dentin treated with
NaOCl for 30 s.
Conclusions: The effects of NaOCl pretreatment on bonding of both self-etch adhesives were
dependent upon type of dentin (normal and caries-affected dentin) and the treatment time.
# 2009 Elsevier Ltd. All rights reserved.

1.

Introduction

Carious dentin consists of two distinct layers (caries-infected


dentin and caries-affected dentin), which have different

morphological and chemical structures. Caries-infected dentin is infected and quite demineralized, and must be removed.
On the other hand, caries-affected dentin is partially demineralized and should be preserved in clinical treatment

* Corresponding author. Tel.: +81 3 5803 5483; fax: +81 3 5803 0195.
E-mail address: genkainada31990326@yahoo.co.jp (G. Taniguchi).
0300-5712/$ see front matter # 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jdent.2009.06.005

770

journal of dentistry 37 (2009) 769775

because it is uninfected and remineralizable. Dental adhesives


are routinely applied to caries-affected dentin after removal of
caries-infected dentin in clinical practice. However, previous
studies have reported that bond strengths to caries-affected
dentin were significantly lower than those to normal dentin16
and the hybrid layer created with caries-affected dentin was
thicker and more porous compared with that with normal
dentin.1,4,6 It was speculated that this was the result of
differences in morphological, biochemical and mechanical
characteristics between normal and caries-affected dentin.7
When the tooth structure is cut, a smear layer is created on
the surface. Surface preparation methods have been shown to
vary the thickness, roughness, density and degree of attachment of the smear layer to the underlying tooth structure.8
Dentin smear layer is composed mostly of submicron particles
of mineralized collagen debris.9,10 It is speculated that there
would be differences in the morphological and chemical
structures of the smear layer created on normal and cariesaffected dentin, because the composition of smear layer is
similar to the underlying dentin substrates.11
Self-etch adhesives are widely used for bonding to enamel
and dentin, because of the simplified bonding procedures and
reduced technique sensitivity.12 Self-etch adhesives are able
to demineralize the smear layer and underlying dentin, while
simultaneously allowing resin monomers to penetrate into
the demineralized zone, which results in the creation of a
hybrid layer.12 However, it has been reported that the
characteristics of the smear layer variously affect the bond
strength of self-etch adhesives to dentin.1316 Therefore, the
characteristics of smear layer covering the caries-affected
dentin might be one reason why self-etch adhesives exhibit
reduced adhesion to caries-affected dentin compared with
normal dentin.
Sodium hypochlorite (NaOCl) solutions are widely used in
the chemomechanical treatment of root canals due to their
antibacterial properties and effective dissolution of organic
substances from biological materials.17 Some researchers
have reported that, when NaOCl was applied to smear
layer-covered dentin, the mineral to matrix ratio at dentin
surface increased and the smear layer was thinned due to
dissolution of the organic phase.18,19 On the other hand, NaOCl
treatment significantly reduces the bond strength to dentin,
since remnants of super-oxide radicals generated by NaOCl
within the dentin surface inhibit polymerization of resin
monomers.2022 In addition, this compromised bonding ability
can be reversed by the application of an antioxidant/reducing
agent prior to the bonding procedures.20,23,24 Recently, the
product, Accel (Sun Medical, Kyoto, Japan), has been introduced for reducing agent, which contains p-toluenesulfinic
acid sodium salt, as a pretreatment before a NaOCl-irrigated
root canal is filled with an adhesive root canal sealer (Super
Bond Sealer, Sun Medical, Kyoto, Japan). However, there is
little published information available on the effect of
pretreatment with NaOCl and reducing agent with regards
to the adhesion of self-etch adhesives to caries-affected
dentin.
The purpose of this study was to evaluate the effect of
pretreatment with NaOCl aqueous solution with or without a
subsequent application of a reducing agent on the adhesion of
one- and two-step self-etch adhesives to normal and caries-

affected dentin and to observe the morphological alterations


of smear layer-covered normal and caries-affected dentin
surfaces after treatment with NaOCl solution. The null
hypothesis tested was that NaOCl pretreatment does not
affect the bond strength to normal and caries-affected dentin
and morphological characteristics of their smear layercovered surfaces.

2.

Materials and methods

Forty extracted human molars with coronal carious lesions,


stored frozen, were used in this study, according to a protocol
approved by the Human Research Ethics Committee, Tokyo
Medical and Dental University, Japan. The inclusion criteria
were that the caries be limited to the occlusal face, that it
extends at least half the distance from the enameldentin
junction to the pulp chamber, and that there is enough
surrounding normal dentin to serve as a control bonding site.
The occlusal enamel was ground perpendicular to the long
axis of the tooth to expose flat surfaces of normal and cariesaffected dentin. In order to obtain caries-affected dentin,
grinding was performed with #600 silicon carbide (SiC) paper
under running water using the combined criteria of visual
examination and staining with a caries-detector solution
(Kuraray Medical, Tokyo, Japan). If, after being bonded and
sectioned, the carious lesion was found to be too shallow or
too deep, the tooth was excluded from this study. After
grinding, the teeth were divided into four groups. The dentin
surfaces of the specimens in group 1 were rinsed with water,
which were served as the control group. For the specimens in
Groups 2 and 3, the dentin surfaces were treated with 6%
NaOCl (Jiaen 6%, Yoshida Co., Tokyo, Japan) for 15 or 30 s,
followed by water rinsing for 10 s. The dentin surfaces of the
specimens in group 4, were treated with 6% NaOCl for 30 s as
previously described, and then treated with Accel (Sun
Medical, Kyoto, Japan) for 30 s, which has a reducing effect,
followed by water rinsing.
After pretreatment, a two-step self-etch adhesive system
(Clearfil Protect Bond; PB; Kuraray Medical, Tokyo, Japan) or onestep self-etch adhesive system (Bond Force; BF; Tokuyama
Dental, Tokyo, Japan) was applied to both normal and cariesaffected dentin according to the manufacturers instructions
(Table 1). Following application of the adhesives, a resin
composite crown was built up using three layers of Clearfil
AP-X (Kuraray Medical, Tokyo, Japan) to a height of 45 mm and
each layer was light cured for 20 s. Then, after storage in tap
water at 37 8C for 24 h, the bonded teeth were vertically
sectioned into four or five 0.7-mm thick slabs using a lowspeed diamond saw (Isomet; Buehler Ltd. Lake Bluff, IL) under
water lubrication. The slight discolored dentin was classified as
caries-affected dentin and the surrounding yellow dentin was
classified as normal dentin with lateral view. Two or three slabs
of bonded normal dentin and two or three slabs of bonded
caries-affected dentin were prepared from per tooth. All the
slabs were hand-trimmed to an hourglass shape with approximately 1 mm2 cross-sectional areas isolated by normal or
caries-affected dentin using a fine diamond bur for the
microtensile bond strength test as previously described.25,26
The final width and thickness of the bonded area were

771

journal of dentistry 37 (2009) 769775

Table 1 Chemical composition and application mode of the materials used in the study.
Material
Clearfil Protect Bond
(PB; Kuraray Medical)
pH; 2.0 (Primer)

Composition

Procedures

Primer: MDP, HEMA, MDPB, dimethacrylates, photo-initiator, water

Apply Primer for 20 s; air dry;


apply Bond; light cure for 10 s

Bond: MDP, HEMA, Bis-GMA, hydrophobicdimethacrylate,


photo-initiators, surface-treated sodium fluoride crystals,
silanated colloidal silica
Bond Force (BF; Tokuyama
Dental) pH; 2.3

Methacryloyloxyalkyl acid phosphate, HEMA, Bis-GMA,


TEGDMA, Glass fillers, Camphorquinone, Isopropyl alcohol, water

Accel (Sun Medical)

p-Toluenesulfinic acid sodium salt ethanol, water

Apply Bond for 20 s; gentle air-dry


and then moderate air-dry more
than 5 s; light cure for 10 s

Abbreviations: MDP: 10-methacryloyloxydecamethylene phosphoric acid; HEMA: 2-hydroxyethyl methacrylate; Bis-GMA: Bis-phenol A
diglydidylmethacrylate; MDPB: 12-methacryloy-loxydodecylpyridinum bromide; TEGDMA: triethyleneglycol dimethacrylate.

measured to the nearest 0.01 mm using a digital micrometer.


The specimens were fixed with cyanoacrylate adhesive (Zapit;
DVA, Anaheim, CA, USA) onto a flat Ciucchis jig attached to a
table-top testing machine (EZ-test; Shimadzu Co., Kyoto, Japan)
and subjected to microtensile testing at a cross-head speed of
1 mm/min. After testing, the modes of failure of the de-bonded
specimens were determined by means of an optical microscope
at 10 and 40 magnifications.

3.

Statistical analysis

The microtensile bond strengths (mTBS) obtained in this study


were analyzed by three-way ANOVA to test the effect of
materials, pretreatment methods and type of dentin (normal
dentin or caries-affected dentin). The Bonferroni and t-test
were used for post hoc multiple comparisons at a = 0.05.

statistically significant interaction between the type of dentin


and the pretreatment method on each adhesive system (PB,
p < 0.001: BF, p = 0.002). For both PB and BF, the mTBS to cariesaffected dentin were significantly lower than those to normal
dentin ( p < 0.05). For normal dentin, NaOCl pretreatment for 30 s
significantly reduced the mTBS of PB and BF ( p < 0.05), while
there were no significant differences in mTBS between the
control and NaOCl-15 s pretreatment groups ( p > 0.05). In
addition, a subsequent application of Accel reversed the
compromised bond strengths to NaOCl-30 s treated dentin. On
the other hand, for caries-affected dentin, the mTBS of PB and BF
after NaOCl pretreatment for 15 s were significantly higher than
those of the no treatment control group ( p < 0.05), while there
were no significant differences in mTBS between the control and
NaOCl-30 s pretreatment groups ( p > 0.05). An application of
Accel increased the mTBS to caries-affected dentin treated with
NaOCl for 30 s. Examination of the failure modes of the all groups
revealed that these were mostly mixed failures in the interface
and cohesive in the adhesive layer and/or dentin (Table 3).

4.
SEM observation of normal and cariesaffected dentin surface after NaOCl pretreatment
6.
Further eight teeth were used for SEM observation. After
treatment with or without NaOCl for 15 and 30 s, the dentin
surface was rinsed off with water and then dehydrated in
ascending concentrations of ethanol in the following steps: 25%
ethanol for 20 min, 50% for 20 min, 75% for 20 min, 95% for
30 min and 100% for 60 min. After the final ethanol step, the
specimens were immersed in hexamethyldisilazane (HMDS) for
10 min, and dried by placement on filter paper inside a covered
glass vial at room temperature for 24 h.19,27 Subsequently, the
dentin surfaces were gold-sputter-coated and observed with a
Scanning Electron Microscope (JXA-840, JEOL, Tokyo, Japan).

5.

Results

The mTBS bond strengths of protect bond (PB) and bond force (BF)
to normal and caries-affected dentin are shown in Table 2.
ANOVA analysis revealed that there was no significant
difference among the materials ( p = 0.32) and there was
significant difference among the pretreatment methods
( p < 0.001) and type of dentin ( p < 0.001) and there was a

SEM observation

In the case of the control group, the smear layer of normal


dentin exhibited a smooth texture with a compact crust of

Table 2 On TBS to normal and caries-affected dentin.


n = 12
Normal dentin

Caries-affected dentin

Protect bond: Mpa mean (SD)


Group 1
40.9 (6.0)ac, p < 0.05
Group 2
42.0 (3.6)ac, NS
Group 3
34.4 (3.5)b, NS
Group 4
37.5 (4.4)bc, NS

27.9
41.6
33.3
39.9

(6.2) A
(6.6) B
(5.2) A
(6.7) B

Bond force: Mpa mean (SD)


Group 1
44.0 (4.0)d, p < 0.05
Group 2
43.7 (9.9)d, NS
Group 3
30.4 (7.7)e, NS
Group 4
36.8 (3.9)de, NS

029.8
040.6
031.4
035.6

(4.6) C
(7.7) D
(8.5) C
(9.1) CD

Same letters indicate statistically no significant differences


( p > 0.05). NS = no significant difference.

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journal of dentistry 37 (2009) 769775

Table 3 Failure modes.


Dentin

Inrerfaciala

Mixedb

Cohesive
In dentinc

Protect Bond
Normal
Group 1
Group 2
Group 3
Group 4
Caries-affected
Group 1
Group 2
Group 3
Group 4
Bond force
Normal
Group 1
Group 2
Group 3
Group 4
Caries-affected
Group 1
Group 2
Group 3
Group 4

In resind

0
0
1
0

10
11
11
10

2
1
0
1

0
0
0
1

1
0
0
0

10
11
10
10

1
1
1
2

0
0
1
0

1
0
1
0

9
10
10
11

0
1
0
0

2
1
1
1

1
0
0
0

9
11
10
10

1
0
1
0

1
1
1
2

Interfacial = 80100% failure occurred between resin and dentin.


Mixed = interfacial failure and cohesive failure in the adhesive
resin and/or dentin.
c
Cohesive failure in dentin = 80100% of the failure occurred in
the underlying dentin.
d
Cohesive failure in resin = 80100% of the failure occurred in the
adhesive resin and/or overlying composite.
b

cutting debris (Fig. 1a), while the caries-affected dentin was


covered with a thicker and irregular smear layer with sludgelike formation, in which fibril-like structures were observed
(Fig. 2a). When NaOCl was applied to the smear layer-covered
normal dentin for 15 and 30 s, alteration in the surface
morphology and smear layer thickness of normal dentin after
15 and 30 s treatment of NaOCl was unclear (Fig. 1b and c). On
the other hand, when the caries-affected dentin was treated
with NaOCl for 15 and 30 s, the smear layer was eroded and
thinned and fibril-like structures were not observed (Fig. 2b
and c). For both normal and caries-affected dentin, there were
no significant alterations in surface morphology between
NaOCl-30 s pretreatment groups and Accel treatment after
NaOCl-30 s pretreatment groups (Fig. 1c and d; Fig. 2c and d).

7.

Discussion

The smear layer on dentin is composed of disorganized


collagen debris binding mineral particles,9,10 and differs little

Fig. 1 Scanning electron micrographs of normal dentin


surface. (a) No treatment. Smear layer was smooth and
compact. (b) Treated with 6% NaOCl for 15 s. There were no
significant alterations in surface morphology from (a). (c)

Treated with 6% NaOCl for 30 s. There were no significant


alterations in surface morphology from (a) and (b). (d)
Treated with 6% NaOCl for 30 s, and then treated with
Accel for 30 s. There were no significant alterations in
surface morphology from (a), (b) and (c). D = dentin.
S = smear layer.

journal of dentistry 37 (2009) 769775

773

in composition from the underlying dentin substrate.11 The


disorganized collagen within the smear layer is not denatured,
however after acidic exposure, it forms a gelatinous matrix
around the mineral.10 The disorganized collagen and/or the
mineral trapped within the gelatinized collagen cannot be
easily removed even when etched with phosphoric acid.28 The
disorganized collagen and the gelatinous layer within the
smear layer may prevent resin monomer infiltration and
prevent a perfect seal at the resindentin interface.10,28
In this study, the smear layer on caries-affected dentin was
thick and irregular with fibril-like structures. On the other
hand, the smear layer on normal dentin was compact with a
smooth surface, in which fibril-like structures could not be
observed. Although dentinal tubules in caries-affected dentin
are occluded by acid-resistant minerals4,29 and are likely to be
impermeable to water,30 the intertubular dentin is partially
demineralized, resulting in it being softer and more porous.
Moreover, the water content of caries-affected dentin
increases as mineral is lost.31 From these results, the smear
layer of caries-affected dentin seems to be enriched with
organic components compared with that of normal dentin.
Furthermore, it might contain acid-resistant minerals.
In this study, the bond strengths of the tested one- and twostep self-etching adhesive systems (Bond Force and Clearfil
Protect Bond) to caries-affected dentin were lower than those
to normal dentin. These results were in agreement with
previous studies.1,2,6 With self-etch adhesives, there is a lower
possibility of smear layer removal because they are less acidic
and have a reduced demineralizing action compared to
phosphoric acid, and incorporate it into the hybrid layer.32
Therefore, for self-etch adhesives, it would be more difficult to
remove the thick and organic-enriched smear layer on the
caries-affected dentin and their organic phase would interfere
with the infiltration of the self-etch adhesive into the underlying dentin, and the porous intertubular dentin, which has a
higher water content, would result in the creation of a poorer
quality hybrid layer that is thick, but gives rise to reduced bond
strengths. Moreover, acid-resistance minerals in the smear
layer on the caries-affected dentin might prevent proper
infiltration of self-etch adhesive into underlying dentin.
Several previous studies have demonstrated that pretreatment of smear layer-covered dentin with NaOCl for 60 s
or a few minutes has a negative effect on bonding.2022 It has
been speculated that reactive residual free-radicals are
present on the NaOCl-treated dentin surface that have been
produced by the oxidizing effect of NaOCl and these compete
with the propagation of vinyl free-radicals generated during
light-activation of the adhesive, resulting in premature chain

Fig. 2 Scanning electron micrographs of caries-affected


dentin surface. (a) No treatment. Dentin surface was

covered with a thick and irregular smear layer in which a


sludge-like formation and fibril like structures were seen
(arrow). (b) Treated with 6% NaOCl for 15 s. The smear
layer was eroded and thinned. Fibril-like structures were
not seen. (c) Treated with 6% NaOCl for 30 s. There were no
significant alterations in surface morphology from (b). (d)
Treated with 6% NaOCl for 30 s, and then treated with
Accel for 30 s. There were no significant alterations in
surface morphology from (b) and (c). D = dentin. S = smear
layer.

774

journal of dentistry 37 (2009) 769775

termination and incomplete polymerization.20 In this study,


NaOCl pretreatment for 30 s significantly reduced the bond
strengths of both self-etch adhesive systems to normal dentin,
while there were no significant differences in mTBS to normal
dentin between the control and NaOCl-15 s treated groups.
However, it was not clear if there were any morphological
alterations of the smear layer-covered dentin surfaces after
NaOCl treatment for 15 and 30 s when the specimens were
observed with the SEM. However, Mountouris et al.18, using
FTIR microspectroscopy, reported that the mineral to matrix
ratio of smear layer-covered dentin surface significantly
increased following NaOCl treatment for 0, 20, 40 and 120 s.
Therefore, the 15 and 30 s treatment time of NaOCl used in this
study seems to be enough to cause an oxidizing effect on a
NaOCl treated-dentin surface. Presumably, in the case of the
NaOCl-15 s treated surface, rinsing off with water for 10 s
could remove the oxidized products from the dentin surface
because there were fewer products and/or a lesser diffusion
depth due to the shorter treatment time, resulting in no
adverse effects on adhesion to dentin. However, in the case of
NaOCl treatment for 30 s, there might be remnants of oxidized
products on the dentin surface after rinsing off with water for
10 s.
On the other hand, in the case caries-affected dentin,
NaOCl pretreatment for 15 s significantly increased the mTBS
of both self-etch adhesives compared with those of the no
treatment groups of caries-affected dentin, and SEM observations clearly indicated that NaOCl pretreatment could dissolve
superficial collagen within the smear layer of caries-affected
dentin, but could not completely remove the smear layer
although it was left thinner. A thinner smear layer on cariesaffected dentin with a reduced organic component might
promote the infiltration self-etch adhesives into the smear
layer and the underlying dentin, leading to higher bond
strengths to caries-affected dentin. When NaOCl was applied
for 30 s, the mTBS of both self-etch adhesives to caries-affected
dentin did not improve and were similar to those of the no
treatment groups of caries-affected dentin. These results
indicate that there were the negative and positive effects of
NaOCl treatment on bonding to dentin; an improvement in
monomer infiltration into dentin due to dissolution of the
organic component in the smear layer and an interference in
resin polymerization due to remaining oxidizing products.
Recently, it has been reported that applying an antioxidant
agent/reducing agent (e.g., sodium ascorbate, sodium thiosulfate solution) resulted in a positive effect when adhesion to
dentin had been compromised by NaOCl.33 In this study,
applying Accel improved the compromised bonding of both
self-etch adhesives to normal dentin treated with NaOCl for
30 s. Accel contains p-toluenesulfinic acid sodium salt. Since
p-toluenesulfinic acid sodium salt solution has a reducing
action, it is possible to reverse the residual oxidizing effects on
a NaOCl-treated dentin surface, resulting in the restoration of
the altered redox potential.20 In the case of caries-affected
dentin, applying Accel after NaOCl treatment for 30 s
increased the mTBS of both self-etch adhesives compared
with the no treatment groups. These results indicate that after
Accel application, the negative effect of the oxidizing effects of
NaOCl on polymerization was reversed and there was a
positive effect on monomer infiltration into caries-affected

dentin due to dissolution of the organic components in the


smear layer by NaOCl.
Durability studies on adhesion to caries-affected dentin are
still limited.5,34 Erhardt et al.34 reported that resin bonded
interfaces to caries-affected dentin were more susceptible to
water degradation when directly exposed than normal dentin
over time. NaOCl pretreatment might improve the quality of
the hybrid layer of caries-affected dentin using self-etch
adhesives due to more infiltration of resin monomer, leading
to more stable bonding to caries-affected dentin. Further
research is required to determine the effect of NaOCl
pretreatment on the bonding durability of caries-affected
dentin, and to evaluate the micromorphologcal structures of
the bonded interface to NaOCl treated caries-affected dentin.

8.

Conclusions

Within the limitations of this study, the bond strengths of the


tested one- and two-step self-etch adhesive systems (Bond
Force and Clearfil Protect Bond), were significantly lower to
caries-affected dentin than normal dentin, in which there were
no significant differences between the adhesive materials. In
addition, the smear layer on caries-affected dentin layer
exhibited a different morphology, which was thick and irregular
with fibril-like structures, compared to the smear layer on
normal dentin, which had a compact surface. The effects of
NaOCl pretreatment on the adhesion of both self-etch adhesives were dependent upon the type of dentin (normal and
caries-affected dentin) and the treatment time. The results
require rejection of the null hypothesis. NaOCl pretreatment for
15 s significantly improved the mTBS of both self-etch adhesives
to caries-affected dentin, while 30 s pretreatment did not affect
them. For normal dentin, NaOCl pretreatment for 30 s significantly reduced the mTBS of both self-etch adhesives
although the 15 s pretreatment did not alter them. NaOCl
treatment of smear layer-covered caries-affected dentin eroded
and thinned the smear layer due to dissolution of superficial
organic components of smear layer, while the morphological
alterations of normal dentin-smear layer were unclear using
scanning electron microscopy. Furthermore, application of the
reducing agent, Accel, increased the mTBS to normal and cariesaffected dentin treated with NaOCl for 30 s.

Acknowledgement
This work was supported by the grant from the Japanese
Ministry of Education, Global Center of Excellence (GCOE)
Program, International Research Center for Molecular
Science in Tooth and Bone Diseases.

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