Japanese Dental Science Review (2011) 47, 102—114

a v a i l a b l e a t w w w. s c i e n c e d i r e c t . c o m

journal homepage: www.elsevier.com/locate/jdsr

Review Article

Bonding to caries-affected dentin

Masatoshi Nakajima *, Sitthikorn Kunawarote, Taweesak Prasansuttiporn,
Junji Tagami

Cariology and Operative Dentistry, Department of Restorative Sciences, Graduate School of Medical and Dental Sciences,
Tokyo Medical and Dental University, 1-5-45 Yushima, Bunkyo-ku, Tokyo 113-8549, Japan

Received 10 December 2010; received in revised form 28 February 2011; accepted 6 March 2011

KEYWORDS Summary Dentin adhesive systems have dramatically developed during the past decades. In a
Caries-affected dentin; prepared cavity for an adhesive composite restoration, large areas of the cavity floor are
Dentin bonding; composed of caries-affected dentin after removal of caries-infected dentin, not normal dentin.
Bond strength; Caries-affected dentin is different in morphological, chemical and physical characteristics from
Adhesive interface normal dentin. Therefore, caries-affected dentin has still problems as bonding substrate com-
pared with normal dentin. That is, caries-affected dentin produces lower bond strength and poor
quality of the hybrid layer than normal dentin. In addition, when exposed the adhesive interface
of caries-affected dentin in oral environment, the poor quality of the hybrid layer would
compromise the longevity of the composite restoration due to hydrolysis of the resin and collagen
fibrils. The improvement of bonding potential to caries-affected dentin could lead to reinforce-
ment of tooth-composite restoration complex, protecting secondary caries and tooth fracture.
# 2011 Japanese Association for Dental Science. Published by Elsevier Ltd. All rights reserved.

Contents

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103
Characteristics of caries-affected dentin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103
Mineral phase . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103
Organic phase . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103
Transparent layer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103
Water content and permeability. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103
Mechanical properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 105
Smear layer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 105
Bonding to caries-affected dentin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 106
Etch and rinse adhesive system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 106
Self-etch adhesive system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 107

* Corresponding author. Tel.: +81 3 5803 5483l; fax: +81 3 5803 0195.
E-mail address: [email protected] (M. Nakajima).

1882-7616/$ — see front matter # 2011 Japanese Association for Dental Science. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.jdsr.2011.03.002
Bonding to caries-affected dentin 103

Bonding durability to caries-affected dentin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109

Effect of caries removal methods on bonding to caries-affected dentin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 113
Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 113
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 113

Introduction crystals are present in remineralized dentin after carious

demineralization, compared to the apatite crystals in intact
Dental caries is the most common pathological change of dentin [17,19]. These indicate that caries-affected dentin
dentin. Fusayama’s research demonstrated that carious den- causes re-precipitation of CO3- and Mg-poor apatite after the
tin consists of two distinct layers: an outer layer of bacte- dissolution of CO3- and Mg-rich apatite [20,21]. Mineral
rially infected dentin, and an inner layer of affected dentin crystals in caries-affected dentin are scattered and randomly
[1]. The outer layer (caries-infected dentin) was character- distributed, with larger apatite crystallites and wider inter-
ized as being highly demineralized, physiologically unremi- crystalline spaces compared with intact dentin [19].
nerazable and showing irreversible denatured collagen fibrils
with a virtual disappearance of cross-linkages. The inner Organic phase
layer (caries-affected dentin) is uninfected, partially demi-
neralized and physiologically remineralizable, therefore The dentin organic matrix contains different extracellular
should be preserved during clinical treatment. Consequently, proteins, such as type I collagen, proteoglycans, dentin
in cavity preparation for an adhesive restoration after phosphoproteins and sialoprotein. Changes in dentin organic
removal of caries-infected dentin, large areas of the cavity matrix associated with caries have been reported [15,22—
floor are composed of caries-affected dentin. Therefore, in 24]. In the inner layer (caries-affected dentin), the general
clinical settings, bonding substrate is commonly caries- pattern of amino acid composition shows no significant dif-
affected dentin, not normal dentin. ferences from intact dentin [22]. In addition, the reducible
Many studies on dentin bonding have used normal dentin intermolecular covalent cross-links of the collagen are partly
as bonding substrate, which have contributed to the dramatic shifted to the precursor form, thus leading to decreased
development of dentin adhesive systems during the past cross-links–—but this change is reversible [22], and the 67-
decades. On the other hand, there is a few study about nm cross-bands of the collagen fibrils remain [23]. These
bonding to caries-affected dentin, in which the bond results support the idea that caries-affected dentin is remi-
strengths to caries-affected dentin are lower than those of neralizable. On the other hand, the secondary structure of
normal dentin [2—13] (Table 1). The inferior bonding efficacy collagen is slightly altered by the carious process [15], and
of caries-affected dentin would affect the clinical perfor- the distribution of antigenically intact collagen fibrils and
mance of adhesive composite restoration. This article dis- proteoglycans is significantly lower in normal dentin [24].
cusses bonding potential to caries-affected dentin and also Reductions in antigenicity from the organic matrix of sclero-
reviews the characteristics of caries-affected dentin. tic dentin under caries lesions raise concern about the
potential of interfibirillar remineralization [24].
Characteristics of caries-affected dentin
Transparent layer
Mineral phase
Under a caries process, continuous deposition of minerals
The mineral phase of dentin is mainly composed of carbo- occurs within the tubule lumen (Fig. 2). In fact, most of the
nate-rich hydroxyapatite. The dentinal caries process con- dentinal tubules in caries-affected dentin are occluded by
sists of dynamic, cyclical episodes of demineralization and mineral crystals [25]. The crystals in the tubule lumen render
remineralization. A Fourier-transform infrared imaging the refractive index of the lumen similar to that of the
(FTIR) study has shown that the mineral phase of caries- intertubular dentin, making the transparent layer. In these
affected dentin is less crystalline and has a lower mineral mineral deposits, Mg was identified although Mg was barely
content than normal dentin [14]. Micro-Raman spectroscopy present in intertubular caries-affected dentin [9]. Therefore,
investigation has suggested that the relative intensity of the intratubular minerals consist of large rhombohedral crystals
mineral carbonate peak at 1070 cm 1 decreased dramati- of Mg-substituted b-TCP (whitlokite) [26], which is less solu-
cally in caries-affected dentin [15]. Electron probe micro- ble than hydroxyapatite.
analysis (EPMA) revealed that caries-affected dentin, as well
as caries-infected dentin showed much lower magnesium Water content and permeability
(Mg) content compared with intact dentin, although the
densities of calcium (Ca) and phosphorus (P) in caries- As mineral is lost from the dentin matrix during the carious
affected dentin were relatively similar to intact dentin [8] process, its volume is replaced by water. The water content
(Fig. 1). The reduction in Mg content in dentin starts before of normal dentin is approximately 10%, whereas that of
the commencement of a decrease in Ca and P content in caries-affected dentin shows a higher value, which varies
dentinal caries [16,17]. Changes in Mg content could be the from 14% to 53% [27]. On the other hand, permeability of
first sign of carious demineralization and may indicate a loss caries-affected dentin decreases due to occlusion of the
of peritubular dentin matrix [18]. Moreover, larger apatite tubules. Tagami et al. [28] found young carious molars were
 104
Table 1 The review papers concerning about bond strength to caries-affected dentin.

Author Ref. Adhesive material Manufacturer Bonding system Bonding Test method Normal dentin Caries-
procedure affected
Nakajima et al. (1995) [2] All Bond 2 Bisco Etch and rinse(wet) 3-Step mTB(hourglass) 26.90 p < 0.05 13.01
Scotchbond Multi-Purpose 3M Etch and rinse(dry) 3-Step 20.32 NS 18.49
Clearfil Liner Bond 2 Kuraray Self-etch 2-Step 29.52 p < 0.05 13.97
Nakajjima et al. (1999) [3] Scotchbond Multi-Purpose 3M Etch and rinse(wet) 3-Step mTB(hourglass) 42.4 NS 48.2
Nakajjima et al. (1999) [4] Clearfil Liner Bond 2 Kuraray Self-etch 2-Step mTB(hourglass) 45.2 p < 0.05 29.7
Clearfil Liner Bond 2V Kuraray Self-etch 2-Step 57.4 p < 0.05 39.1
ART Bond Coltene Self-etch 2-Step 24.9 NS 30.2
Yoshiyama et al. (2000) [5] FluoroBond Shofu Self-etch 2-Step mTB(hourglass) 28.2 p < 0.05 17.5
Single Bond 3 M ESPE Etch and rinse(wet) 2-Step 46.0 p < 0.05 27.1
Single Bond Etch and rinse(dry) 2-Step 26.4 p < 0.05 18.1
Yoshiyama et al. (2002) [6] ABF (Clearfil Protect Bond) Kuraray Self-etch 2-Step mTB(dumbbell) 44.9 p < 0.05 25.3
Single Bond 3 M ESPE Etch and rinse 2-Step 50.9 p < 0.05 28.8
Ceballos et al. (2003) [7] Prime and bond NT Dentsply Etch and rinse 2-Step mTB(hourglass) 56.3 p < 0.05 41.3
Scotchbond 1 3 M ESPE Etch and rinse 2-Step 43.9 NS 36.3
Clearfil SE Bond Kuraray Self-etch 2-Step 35.5 p < 0.05 21.5
Adper Prompt L Pop 3 M ESPE Self-etch 1-Step 18.2 NS 13.4
Doi et al. (2004) [8] Clearfil SE Bond Kuraray Self-etch 2-Step mTB(hourglass) 41.2 p < 0.05 21.5
Mac-Bond II Tokuyama Self-etch 2-Step 35.0 p < 0.05 20.2
Unifil Bond GC Self-etch 2-Step 27.2 p < 0.05 19.6
Nakajima et al. (2005) [9]] Clearfil Protect Bond Kuraray Self-etch 2-Step mTB(hourglass) 43.5 p < 0.05 29.4
Say et al. (2005) [10] Optibond Solo Plus Kerr Etch and rinse 2-Step mTB(hourglass) 38.7 p < 0.05 28.5
Total-etch (photo-cure)
Optibond Solo Plus Self-etch 2-Step 44.2 p < 0.05 29.2
Self-etch (photo-cure)
Optibond Solo Plus Etch and rinse 2-Step 17.2 p < 0.05 10.5
Total-etch (dual-cure)
Optibond Solo Plus Self-etch 2-Step 18.3 p < 0.05 13.5
Self-etch (dual-cure)
Pereira et al. (2006) [11] Single Bond 3 M ESPE Etch and rinse 2-Step mTB(hourglass) 43.3 NS 36.1
Adper Prompt L Pop 3 M ESPE Self-etch 1-Step 52.0 p < 0.05 37.3

M. Nakajima et al.
Wei et al. (2008) [12] Clearfil SE Bond Kuraray Self-etch 2-Step mSB 44.96 p < 0.05 33.76
Clearfil Tri-S Bond Kuraray Self-etch 1-Step 40.48 p < 0.05 33.3
Single Bond 3 M ESPE Etch and rinse 2-Step 44.69 p < 0.05 32.65
Scholt anus et al. (2010) [13] Scotchbond 1XT 3 M ESPE Etch and rinse 2-Step mTB(bar) 35 p < 0.05 25
Clearfil Tri-S Bond Kuraray Self-etch 1-Step 35 p < 0.05 21
Clearfil SE Bond Kuraray Self-etch 2-Step 33 NS 39
Bonding to caries-affected dentin 105

Figure 1 Light microscopic photographs and EPMA mapping images of carious tooth [9]. (A) Cross-sectioned specimen of carious
tooth; (B) specimen A stained by caries detector solution; (C) mapping images of elemental distribution (Ca, P, Mg) and backscatter
electronic image of specimen A observed by EPMA. Mg-depleted area corresponds well to the morphological changes seen in light
microscope images (A and B).

only 14% as permeable as young normal dentin and suggested the Knoop hardness number [6]. On the other hand, Nishitani
that the transparent layer would be effective in decreasing et al. [32] reported that the matrix of demineralized caries-
permeability. affected dentin was as strong as that of normal deminer-
alized dentin. These results would indicate that lower UTS
Mechanical properties and hardness of caries-affected dentin are due to loss of
mineral in intertubular dentin. Marshall et al. [29] reported
Caries-affected dentin is softer than normal dentin, with that the mean elastic modulus (18.2 GPa) and nanohardness
about half the hardness, even though mineral depositions (0.8 GPa) of intertubular dentin on the transparent layer
occlude dentinal tubules [2,7,11,25,29—31]. In addition, were slightly, but significantly lower than those of the unaf-
ultimate tensile strength (UTS) of caries-affected dentin is fected intertubular dentin (20.6 and 1.0 GPa, respectively).
also lower than that of normal dentin, and there is a positive On the other hand, for arrested caries, the elastic modulus of
correlation in caries-affected dentin between the UTS and the transparent layer of caries-affected dentin is not sig-
nificantly different from the underlying normal dentin
although its hardness is lower than normal dentin [30,31].

Smear layer

Cavity preparation with rotary instruments or others results

in the formation of a smear layer on the dentin surface, in
which the cutting method affects smear layer characteristics
(i.e. thickness, density). The smear layer fills the orifices of
dentinal tubules, to form smear plugs, leading to a reduction
in dentin permeability. However, sub-micron porosities in the
smear layer still allow for the diffusion of dentinal fluid. The
dentin smear layer with smear plugs is composed mostly of
submicron particles of mineralized collagen debris [33,34],
which differs little in composition from the underlying dentin
[33—35]. Therefore, the smear layer formed on caries-
affected dentin would be different in morphological and
chemical structures from that of normal dentin, because
Figure 2 Scanning electron micrograph (SEM) of the transpar- caries-affected dentin is partially demineralized, leading
ent layer of caries-affected dentin [28]. Many mineral casts to different mineral/organic contents compared to normal
occludes dentinal tubules. dentin. Indeed, the smear layer of caries-affected dentin is
106 M. Nakajima et al.

Figure 3 Schematic illustration of smear layers of normal and caries-affected dentin. Caries-affected dentin smear layer is thick with
enriched organic components compared with normal dentin smear layer.

thicker and appears to be enriched with organic components matrix. In addition, a larger quantity of water in the deeper
compared with that of normal dentin (Fig. 3) [36,37]. demineralized zone would compete with penetration of the
adhesive resin monomers. Besides the residual water, caries-
Bonding to caries-affected dentin affected dentin may contain substances that interfere with
free radical generation or propagation, leading to poor poly-
merization of adhesive monomers. It is reported that the
Caries-affected dentin produces lower bond strengths than
degree of conversion of adhesive agent that penetrated the
normal dentin, regardless of the type of adhesive system
etched dentin in the caries-affected dentin specimen was
(etch and rinse system or self-etch system; one-, two- or
lower than in the normal dentin specimens [14].
three-step of bonding procedure) [2—13,36—39], in which
The mineral deposits in dentinal tubules in the transpar-
cohesive failure of specimens in dentin increases in resin-
ent layer are highly acid resistance. Etching with phosphoric
bonded caries-affected dentin [6,7,10]. A reduction in the
acid cannot completely dissolve the deposits that exist in
cohesive strength of caries-affected dentin would be one of
dentinal tubules without dissolution. The presence of mineral
the reasons for lower bond strength values to caries-affected
deposits inside dentinal tubules would interfere with resin
dentin compared with normal dentin [6]. On the other hand,
monomer infiltration peripheral to the dentinal tubules as
Wei et al. [12] demonstrated that when analyzing the effect
well as resin tag formation, leading to lower bond strength
of dentin type (normal and caries-affected dentin) on bond
[2,5].
strength after removing the variance for which hardness
The hybrid layer of etch and rinse system in caries-
accounted as a covariate, it was found that the condition
affected dentin was thicker but susceptible to the acid
of dentin had a significant effect on bond strength: even if
and base treatment in scanning electron microscopy (SEM)
normal and caries-affected dentin had similar intertubular
observation of resin/caries-affected dentin interface [2]
hardness, bond strength to caries-affected dentin would still
(Fig. 4). Transmission electron microscopy (TEM) observation
be significantly lower than to normal dentin. The change in
demonstrated a more porous zone along the base of the
chemical and morphological characteristics of caries-
hybrid layer in caries-affected dentin created [6]. Micro-
affected dentin would be also reasons for the lower bond
Raman spectroscopy investigation suggested that the car-
strength. The hybrid layers created to caries-affected dentin
ies-affected dentin interface was more complicated,
are thicker than those of normal dentin, because caries-
whereby the wider demineralized matrix was not protected
affected dentin is more susceptible to the acid etching
by the critical Bis-GMA [15]. Light microscopy evaluation with
due to partially demineralization, resulting in the formation
Masson’s trichrome stain indicated wider regions of non-
of a deeper demineralized zone [2—6,8—10,15,38,40].
encapsulated collagen in the caries-affected dentin interface
[40]. These would be due to reduced penetration of the resin
Etch and rinse adhesive system monomers into the etched caries-affected dentin because of
the deeper demineralized zone and the presence of the
When phosphoric acid etchants are applied to normal and mineral deposits inside the dentinal tubules (Fig. 5).
caries-affected dentin surface, the smear layer is completely Etching with phosphoric acid might be too aggressive for
removed, and both dentinal sub-surfaces are demineralized partially demineralized intertubular caries-affected dentin.
and the collagen fibrils are exposed. In order to produce a However, stronger acids and an extended etching time are
superior resin—dentin interface, resin monomers must pene- suggested for solubilizing acid resistant mineral deposits
trate into these demineralized dentinal sub-surfaces. How- within the caries-affected tubule lumens, leading to more
ever, even though for normal dentin, it has been lateral penetration of the adhesive monomer from the tubule
demonstrated that there are discrepancies between the lumens. When One-Step (Bisco) with 10% phosphoric acid
depths of demineralization and resin monomer penetration. etchant was applied to caries-affected dentin, it resulted
The wet bonding technique is effective for infiltration of resin in lower bond strength than normal dentin, however this
monomers into deeper acid-etched demineralized layers in significant difference disappeared following the application
caries-affected dentin compared with the dry bonding tech- of 32% phosphoric acid [38]. Arrais et al. [39] reported that
nique, leading to higher bond strength [4,5]. Nevertheless, a extending the etching time for 35% phosphoric acid from 15 s
deeper demineralized zone is more difficult for resin mono- to 45 s duration improved the bond strength of Single Bond
mer to penetrate to the bottom of the exposed collagen (3M ESPE) to caries-affected dentin. However, its bond
Bonding to caries-affected dentin 107

Figure 4 Scanning electron micrographs (SEM) of dentin specimens bonded with all bond 2 after acid and base challenge [2]. (A)
Normal dentin: the hybrid layer is about 3—4 mm thick and was resistant to acid/base challenge; (B) caries-affected dentin: the hybrid
layer is 5—7 mm thick The middle of the hybrid layer was partially removed by acid/base challenge. Tube-like structures of the resin
tags would indicate presence of residual mineral casts before acid/base challenge. R = resin; H = hybrid layer; D = dentin.

Figure 5 Schematic illustration of interface of normal and caries-affected dentin using etch and rinse adhesive. The mineral deposits
in dentinal tubules interfere with resin monomer infiltration peripheral to the dentinal tubules as well as resin tag formation. Caries-
affected dentin produces thicker hybrid layer, in which there are poorer infiltrations of resin monomers into etched dentin because of
the deeper demineralized zone and the presence of the mineral deposits inside the dentinal tubules.

strength was still lower than that of normal dentin. Since a penetration occur simultaneously. However, TEM observation
longer etching time would deepen the zone of demineralized revealed a porous zone beneath the hybrid layer of self-etch
intertubular dentin, the discrepancy between the deminer- system in caries-affected dentin [6]. Nakajima et al. [9]
alized layer and resin monomer penetration could not be reported that there was a thicker nitrogen-rich layer at
eliminated. the caries-affected dentin interface of 2-step self-etch sys-
Recently, the application of chemical cross-linker in the tem using EPMA analysis, which is indicative of a collagen-
bonding procedures has been introduced, which may poten- rich phase (Fig. 6). Light microscopy evaluation with Masson’s
tially increase dentin collagen stability due to a higher trichrome stain indicated wider regions of non-encapsulated
number of collagen cross-linkages [41]. When etch and rinse collagen in the caries-affected dentin interface of 1-step and
systems (One-step Plus, Bisco; Single Bond Plus, 3M ESPE) 2-step self-etch systems [40]. These results indicate that
were used, application with the chemical cross-linking self-etch adhesives could not fully infiltrate adhesive mono-
agents (glutaraldehyde and grape seed extract) for 1 h after mers into the demineralized zone in caries-affected dentin.
acid etching significantly improved bond strength to caries- Self-etch system cannot dissolve and remove acid-resis-
affected and sound dentin, in which the cross-linked dentin tant mineral deposits in dentinal tubules of caries-affected
matrix might mechanically strengthen incomplete resin- dentin because of their higher pH. Therefore, an etch and
infiltrated demineralized zone at the bottom of the hybrid rinse adhesive system using 30—35% phosphoric acid with
layer [41]. stronger acidity might have the upper hand compared with
self-etch systems, although phosphoric acid etching could
Self-etch adhesive system not completely dissolve the mineral deposits in dentinal
tubules in caries-affected dentin. However, using the same
Self-etch systems have also exhibited lower bond strengths to bonding agent of Optibond Solo Plus (Kerr), a total-etch
caries-affected dentin than normal dentin, and their hybrid technique with phosphoric acid did not have any beneficial
layers in caries-affected dentin are also thicker than those of effect on caries-affected dentin compared with the self-etch
normal dentin but absolutely thinner than those of etch and technique [10]. Even though for normal dentin, the mild
rinse systems [2,6,10,40]. Using self-etch adhesives, it has acidity of self-etch systems is not sufficiently effective in
been generally accepted that there are fewer discrepancies the dissolution of smear plugs, therefore smear plugs are
between depths of demineralized zone and resin monomer retained in the dentinal tubules as part of the hybridized
penetration, because demineralization and resin monomer complex with less resin tag formation. In this situation,
108 M. Nakajima et al.

with that of normal dentin [36,37]. The disorganized collagen

and/or the mineral trapped within the gelatinized collagen
cannot be easily removed even when etched with phosphoric
acid [43]. The disorganized collagen and the gelatinous layer
within the smear layer may hinder resin monomer infiltration
and prevent a perfect seal at the resin—dentin interface
[34,43]. Therefore, the caries-affected dentin smear layer
enriched with organic components would contribute to the
inferior adhesion of self-etch adhesives to caries-affected
dentin (Fig. 7).
Sodium hypochlorite solution (NaOCl) can effectively dis-
solve organic substrates from biological materials. Taniguchi
et al. [36] demonstrated that 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 (Fig. 8). Furthermore, they reported that pre-
treatment with 6% NaOCl for 15 s could significantly improve
the bond strengths of 1-step and 2-step self-etch system to
Figure 6 EPMA line analysis of Ca, P, Mg, and N at the adhesive
caries-affected dentin, while NaOCl-30 s pretreatment did not
interface of Clearfil Protect Bond [9]. (a) Normal dentin; (b)
affect them [36]. On the other hand, for normal dentin, NaOCl-
caries-affected dentin. N peaks were observed in the deminer-
15 s pretreatment did not alter the bond strengths, but NaOCl-
alized zones in both interfaces. An increase in N content oc-
30 s pretreatment reduced them [36]. It has been speculated
curred from the interface, peaked then decreased to a level
that applying NaOCl for 30 s or longer results in reactive
similar to that of the underlying dentin. Demineralized zones in
residual free-radicals being present on the NaOCl-treated
normal dentin and caries-affected dentin were 3.5 and 7 mm
dentin that have been produced by the oxidizing effect of
thick, respectively. D = dentin; A = adhesive resin; T = dentinal
NaOCl and these compete with the propagation of vinyl free-
tubule. The line analysis was performed in two white line.
radicals generated during light activation, resulting in pre-
mature chain termination and incomplete polymerization
lateral penetration of the adhesive monomers from the [44]. Applying a reducing agent (Accel; p-Toluenesulfinic acid
dentinal tubules could not contribute to hybrid layer forma- sodium salt: Sun Medical) is effective in recovering the nega-
tion of self-etch adhesives. Therefore, for self-etch systems, tive effect of NaOCl-oxidized dentin for 30 s on polymeriza-
the presence of mineral deposits in dentinal tubules would tion, leading to increased bond strengths to normal and caries-
not be an important reason why caries-affected dentin affected dentin [36]. Kunawarote et al. [37] reported the
causes less penetration of adhesive monomers, leading to application of a mild acidic HOCl solution (Comfosy: Haccpper
lower bond strength than normal dentin, but a deeper miner- Advantec) as a pretreatment agent instead of NaOCl solution.
alized zone would be the main reason. On the other hand, in Mild acidic HOCl solution is an antiseptic and an irrigant, which
the case of self-etch systems, the dentin smear layer would has outstanding properties because not only does it exhibit
affect penetration of the adhesive monomers into the under- biocompatibility and low cytotoxicity but also has immediate
lying dentin. and highly effective antimicrobial and deproteinizing proper-
Several studies using normal dentin have demonstrated ties. The 5 s pretreatment with 50 ppm Comfosy significantly
that dentin smear layer characteristics have been reported improved the bond strengths of 2-step self-etch system to
to compromise the bonding efficacy of self-etch systems. The caries-affected dentin, but the 5 s pretreatment with 6%
smear layer on dentin is composed of disorganized collagen NaOCl did not affect them [37]. Pretreatment with mild acidic
debris binding submicron mineral particles [33,34]. The smear HOCl solution could be able to improve the quality of the
layer of caries-affected dentin is thick and irregular, and hybrid layer of caries-affected dentin created by self-etching
appears to be enriched with organic components compared adhesives due to removal of disorganized/gelatinized collagen

Figure 7 Schematic illustration of interface of normal and caries-affected dentin using self-etch adhesive. The gelatinized collagen
in smear layer is not completely removed, forming hybridized smear layer. The thick gelatinous layer of caries-affected dentin smear
layer would hinder resin monomer infiltration into underlying demineralized zone, resulting in poorer quality of the hybrid layer.
Bonding to caries-affected dentin 109

Figure 8 Scanning electron micrographs (SEM) of the #600 SiC-paper ground normal (A) and caries-affected dentin (B) surfaces [36].
(a) No treatment; (b) treated with 6% NaOCl for 15 s; (c) treated with 6% NaOCl for 30 s. For normal dentin, smear layer was smooth and
compact. There were no significant alterations in surface morphological form. For caries-affected dentin, dentin surface was covered
with a thick and irregular smear layer with sludge-like formation in which fibril-like structures were seen. After treatment with NaOCl,
the smear layer was eroded and thinned in which fibril-like structures were not seen.

and enhancement of resin monomer penetration (Figs. 9 and [40,45—47] (Table 3). Erhardt et al. [40] reported that caries-
10), leading to more stable bonding to caries-affected dentin affected dentin reduced the bond strengths regardless of the
in long term (Table 2). adhesive systems after direct exposure of the interface to
water for 6 months. They indicated that the bonded inter-
faces of caries-affected dentin are more prone to hydrolytic
Bonding durability to caries-affected dentin degradation than those of normal dentin. Recently, Pashley
et al. [48], demonstrated that host-derived matrix metallo-
Adhesive restorations are exposed to a severe environment in proteinases (MMPs) enzymes in the dentin matrix promote
the oral cavity. Occlusal stress, thermal stress and chemical the degradation of exposed, unprotected collagen within
attack by acid and enzymes affect the adhesive interface, incompletely resin-infiltrated acid-etched dentin. The use
compromising the integrity of adhesive restoration. A known of MMP inhibitor such as chlorhexidine, after acid etching,
degradation factor of resin—dentin bond is exposure to could prevent and minimize the degradation of exposed
water. The exposed, altered collagen fibrils at the resin— collagen within incompletely resin-infiltrated hybrid layers,
dentin interface would be susceptible to further collagen contributing to the long-term stability of the hybrid layer and
disorganization or denaturation in the direct water exposure, bond strength. Komori et al. [45] reported that chlorhexidine
leading to degradation of the bonded interface. Durability treatment for 60 s after acid etching significantly lowered
studies on bonding to caries-affected dentin are still limited loss of bond strengths of etch and rinse systems to normal
 110
Table 2 The review paper concerning about improvement effect on bonding to caries-affected dentin.

Author Ref. Adhesive Manufacturer Bonding Bonding procedure Test method Normal Caries-
material system dentin affected
Nakajima [38] One-step Bisco Etch and 32% H3PO4 Bond mTB(hourglass) 49.7 NS 45.2
et al. (2000) rinse
10% H3PO4 Bond 47.7 p < 0.05 36.9
Single Bond 3 M ESPE Etch and 35% H3PO4 Bond 49.5 p < 0.05 40.2
rinse
10% H3PO4 Bond 51.7 p < 0.05 41.2
Arrrais [39] Clearfil Kuraray Self-etch Self-etching primer Bond mTB(hourglass) 41.82 p < 0.05 23.06
et al. (2004) SE Bond
H3PO4 etching + Bond 48.70 p < 0.05 30.76
self-etching primer
Single Bond 3 M ESPE Etch and H3PO4 Bond 50.69 p < 0.05 23.58
rinse
Extending H3PO4 Bond 43.74 p < 0.05 33.97
etching for 45 s
Erhardt [42] Scotchbond 1 3 M ESPE Etch and H3PO4 Bond mTB(hourglass) 31.9 p < 0.05 26.2
et al. (2008) rinse
EDTA Bond 28.1 NS 24.9
H3PO4 + chlorhexidine Bond 27.3 NS 23.8
Taniguchi [36] Clearfil Kuraray Self-etch Self-etching primer Bond mTB(hourglass) 40.9 p < 0.05 27.9
et al. (2009) Protect Bond
NaOCl (15 s) Self-etching primer Bond 42.0 NS 41.6
NaOCl (30 s) Self-etching primer Bond 34.3 NS 33.3
NaOCl (30 s) Self-etching primer Bond 37.5 NS 39.9
+ accel
Bond Force Tokuyama Self-etch Bond 44.0 p < 0.05 29.8
NaOCl (15 s) Bond 43.7 NS 40.6
NaOCl (30 s) Bond 30.4 NS 31.4
NaOCl (30 s) Bond 36.8 NS 35.6
+ accel
Macedo [41] Single 3 M ESPE Etch and H3PO4 Bond mTB(beam) 59.62 p < 0.05 36.75
et al. (2009) Bond Plus rinse
H3PO4 + glutaraldehyde Bond 71.89 p < 0.05 55.55
H3PO4 + grape seed Bond 68.34 p < 0.05 55.9

M. Nakajima et al.
extract
One-Step Bisco Etch and H3PO4 Bond 65.22 p < 0.05 37.38
Plus rinse
H3PO4 + glutaraldehyde Bond 74.30 p < 0.05 57.18
Bonding to caries-affected dentin 111
52.85

26.77

31.62
39.28
34.16
p < 0.05

p < 0.05

p < 0.05

p < 0.05
NS
73.14

41.26

40.34
41.97
41.24
mTB(hourglass)
Bond

Bond

Bond
Bond
Bond
Self-etching primer

Self-etching primer
Self-etching primer
Self-etching primer
H3PO4 + grape seed

Figure 9 Transmission electron micrograph (TEM) of the adhe-

sive interface of Clearfil SE Bond in caries-affected dentin. The
interface exhibited irregular with thicker and more porous
extract

hybrid layer, in which hybridized smear layer was seen with

the ‘‘fuzzy carpet’’ appearance along the top of the hybrid layer.
HOCl 100 ppm (5 s)
HOCl 50 ppm (5 s)
NaOCl (5 s)
Self-etch
Kuraray
SE Bond
Clearfil
[37]
et al. (2011)
Kunawarote

Figure 10 Transmission electron micrograph (TEM) of the

adhesive interface of Clearfil SE Bond in caries-affected dentin
pretreated with 50 ppm HOCl solution for 5 s. The hybrid layer
was thinner and uniform without hybridized smear layer.
 112
Table 3 The review papers concerning about bonding durability to caries-affected dentin.

Author Ref. Adhesive Manufacturer Bonding Bonding Test method Degradation Normal dentin Caries-affected dentin
material system procedure stress
Nakajima [47] mTB Storage with 24 h 1 month 24 h 1 month
et al. (hourglass) hydrostatic
(2006) pulpal pressure
Clearfil Kuraray Self-etch 2-Step 47.3 p < 0.05 29.4 31.4 NS 28.3
SE Bond
Omar [46] mTB(stick) Thermocycling Before After Before After
et al.
(2007)
Scotchbond MP 3M Etch and 3-Step 22.19 p < 0.05 15.7 18.6 NS 16.62
rinse
Clearfil SE Bond Kuraray Self-etch 2-Step 24.25 NS 22.3 20.7 NS 20.23
Xeno IV Dentsply/ Self-etch 1-Step 21.43 NS 18.3 15.45 NS 14.8
Caulk
Erhardt [40] mTB Storage in 24 h 6 months 24 h 6 months
et al. (hourglass) water
(2007)
Scotchbond 1 3M Etch and 2-Step 42.6 NS 38.4 34.5 p < 0.05 27.8
rinse
Clearfil Protect Kuraray Self-etch 2-Step 39.2 NS 39.5 28.7 p < 0.05 24.5
Bond
AdheSE Ivoclar Self-etch 2-Step 28.2 NS 27.2 24.2 p < 0.05 17.2
Vivadent
Komori [45] mTB(beam) Storage in 24 h 6 months 24 h 6 months
et al. artificial
(2009) saliva
a a a a
Scotchbond MP 3 M ESPE Etch and 3-Step p < 0.05 NS
rinse
a a a a
Scotchbond MP NS NS
with 2%CHX
a a a a
Single Bond 2 3 M ESPE Etch and 2-Step p < 0.05 p < 0.05

M. Nakajima et al.
rinse
a a a a
Single Bond 2 p < 0.05 NS
with 2%CHX
Bonding to caries-affected dentin 113

dentin after 6-month storage in artificial saliva, but it did not be influenced by the caries-removal method in conjunction
alter the bond strength of caries-affected dentin. with the adhesive system used.
Thermocycling showed no significant effects on the bond
strength of 3-step etch and rinse system to caries-affected Conclusion
dentin, although there were significant reductions in bond
strength to sound dentin. Moreover, for 1-step and 2-step
Caries-affected dentin is very different in morphological,
self-etch adhesives, no significant effect on bond strength
chemical and physical characteristics from normal dentin.
was detected when bonded to sound and caries-affected
Clinically, resin composite is bonded into a prepared cavity
dentin [46].
after removal of caries-infected dentin, in which the cavity
Fluid penetration into the resin—dentin interface occurs
floor commonly consists of caries-affected dentin with lower
via dentinal tubules under constant hydrostatic pulpal pres-
bonding efficacy. The intrinsic weakness of caries-affected
sure, as well as via the dentin margin. Therefore, the pre-
dentin may not be a clinical problem, if there is surrounding
sence of mineral deposits in dentinal tubules may alter the
normal dentin and/or enamel that can provide high bond
bonding durability between normal and caries-affected den-
strength to the adhesives [6]. However, given that adhesion
tin. Nakajima et al. [47] reported that constant hydrostatic
to the cavity floor is strongly influenced by the contraction
pulpal pressure during 1-month storage significantly
stress of the resin composite, low bonding efficacy to caries-
decreased the bond strength of 2-step self-etch system to
affected dentin would cause further deterioration of the
normal dentin, but did not affect the bond strength to caries-
adhesive interface at the cavity floor in the restored cavity.
affected dentin. The lower dentin permeability of caries-
In addition, when exposed the adhesive interface of caries-
affected dentin may therefore reduce water penetration into
affected dentin in oral environment, the poor quality of the
the interface, leading to long-term stability of the interface
hybrid layer of caries-affected dentin would compromise the
when there is no direct exposure to water in presence of the
longevity of the composite restoration due to hydrolysis of the
surrounding bonded enamel. Tubular occlusion may prevent
resin and collagen fibrils. The specific composition in adhesives
water entrapment, being manifestations of evaporative and
may affect bonding to caries-affected dentin. However,
convective water flux from dentin, at the resin—dentin inter-
improvement effect of composition in adhesives on bonding
face [49]. Current one-step self-etch adhesives show higher
to caries-affected dentin is unclear. One study [3] compared
hydrophilicity, and attract water from the hydrated dentin
the bond strengths of Scotchbond Multi-Purpose (3M) with and
substrate during application on the adhesive surface and
without polyalkenoic acid copolymer in the primer. It was
absorb water even after polymerization. Ultrastructurally,
reported that the polyalkenoic acid in the primer contributed
water entrapment in the 1-step self-etch adhesive layer is
to high bond strength to caries-affected dentin [3]. The
observed in the bonded normal dentin specimen as water-
improvement of bonding potential to caries-affected dentin
filled channels (i.e. water-tree, water-droplet), however
should be considered in new development strategies of adhe-
water-treeing and water-droplet formation can be elimi-
sive materials and carious treatment, which could lead to
nated in the bonded caries-affected dentin specimen [49].
reinforcement of tooth-composite restoration complex, pro-
In the absent of water fluxes from caries-affected dentin, a
tecting secondary caries and tooth fracture.
one-step self-etch adhesives might initially establish a better
seal along the interface. However, the absorbed water in the
adhesive layer would cause hydrolytic degradation of resi- References
nous materials over time, compromising the integrity of the
resin—dentin interface. [1] Fusayama T. Two layers of carious dentine: diagnosis and treat-
ment. Oper Dent 1979;4:63—70.
[2] Nakajima M, Sano H, Burrow MF, Tagami J, Yoshiyama M, Ebisu S,
Effect of caries removal methods on bonding Ciucchi B, Russel CM, Pashley DH. Tensile bond strength and SEM
to caries-affected dentin evaluation of caries-affected dentin using dentin adhesives. J
Dent Res 1995;74:1679—88.
Some researchers have evaluated the effect of caries removal [3] Nakajima M, Sano H, Zheng L, Tagami J, Pashley DH. Effect of
moist vs dry bonding to normal vs. caries-affected dentin using
method on bonding to caries-affected dentin [50,51]. Using
scotchbond multi-purpose plus. J Dent Res 1999;78:1298—303.
etch and rinse system of Single Bond (3M), caries removal [4] Nakajima M, Ogata M, Okuda M, Tagami J, Sano H, Pashley DH.
methods (steel bur in a slow-speed handpiece, air abrasion Bonding to caries-affected dentin using self-etching primers.
with aluminum oxide particle, partially diamond-coated oscil- Am J Dent 1999;12:309—14.
lating tip with airscaler, hand excavator with Carisolv) did not [5] Yoshiyama M, Urayama A, Kimochi T, Matsuo T, Pashley DH.
affect the bond strength to caries-affected dentin [50]. This Comparison of conventional vs self-etching adhesive bonds to
result is in agreement with another study using etch and rinse caries-affected dentin. Oper Dent 2000;25:163—9.
system of OptiBond Solo Plus Total-Etch (Kerr), in which there [6] Yoshiyama M, Tay FR, Doi J, Nishitani Y, Yamada T, Itou K, Carvalho
were no significant differences in bond strength to caries- RM, Nakajima M, Pashley DH. Bonding of self-etch and total-etch
affected dentin between excavation by a steel round bur in a adhesives to carious dentin. J Dent Res 2002;81:556—60.
[7] Ceballos L, Camejo DG, Fuentes MV, Osorio R, Toledano M,
slow-speed handpiece, Er:YAG laser and 600-grit SiC paper
Carvalho RM, Pashley DH. Microtensile bond strength of total-
[51]. On the other hand, in this study, the 2-step self-etching etch and self-etching adhesives to caries-affected dentine. J
system of Clearfil Protect Bond (Kuraray Medical) exhibited Dent 2003;31:469—77.
lower bond strength to caries-affected dentin excavated by [8] Doi J, Itota T, Torii Y, Nakabo S, Yoshiyama M. Micro-tensile bond
steel round bur than Er:YAG laser and 600-grit SiC paper. These strength of self-etching primer adhesive systems to human
results indicate that adhesion to caries affected dentin might coronal carious dentin. J Oral Rehabil 2004;31:1023—8.
114 M. Nakajima et al.

[9] Nakajima M, Kitasako Y, Okuda M, Foxton RM, Tagami J. Ele- [32] Nishitani Y, Yoshiyama M, Tay FR, Wadgaonkar B, Waller J, Agee
mental distributions and microtensile bond strength of adhesive K, Pashley DH. Tensile strength of mineralized/demineralized
interface to normal and caries-affected dentin. J Biomed Mater human normal and carious dentin. J Dent Res 2005;84:1075—8.
Res B Appl Biomater 2005;72B:268—75. [33] Pashley DH, Ciucchi B, Sano H, Horner JA. Permeability of dentin
[10] Say EC, Nakajima M, Penawongse P, Soyman M, Ozer F, Tagami J. adhesive agents. Quintessence Int 1993;24:618—31.
Bonding to sound vs caries-affected dentin using photo- and [34] Spencer P, Wang Y, Walker MP, Swafford JR. Molecular structure
dual-cure adhesives. Oper Dent 2005;30:90—8. of acid-etched dentin smear layers–—in situ study. J Dent Res
[11] Pereira PNR, Numes MF, Miguez PA, Swift Jr EJ. Bond strength of 2001;80:1802—7.
a 1-step self-etching system to caries-affected and normal [35] Ruse ND, Smith DC. Adhesion to bovine dentin—surface charac-
dentin. Oper Dent 2006;31:677—81. terization. J Dent Res 1991;70:1002—8.
[12] Wei S, Sadr A, Shimada Y, Tagami J. Effect of caries-affected [36] Taniguchi G, Nakajima M, Hosaka K, Iwamoto N, Ikeda M, Foxton
dentin hardness on the shear bond strength of current adhe- RM, Tagami J. Improving the effect of NaOCl pretreatment on
sives. J Adhes Dent 2008;10:431—40. bonding to caries-affected dentin using self-etch adhesives. J
[13] Scholtanus H, Purwanta K, Dogan N, Kleverlaan CJ, Feilzer AJ. Dent 2009;37(10):769—75.
Microtensile bond strength of three simplified adhesive systems [37] Kunawarote S, Nakajima M, Foxton RM, Tagami J. Pretreatment
to caries-affected dentin. J Adhes Dent 2010;12:273—8. effect of mild acidic HOCl solution on adhesive to caries-affect-
[14] Spencer P, Wang Y, Katz JL, Misra A. Physicochemical interac- ed dentin using self-etch adhesive. Eur J Oral Sci 2011;119(1):
tions at the dentin/adhesive interface using FTIR chemical 86—92.
imaging. J Biomed Opt 2005;10(3):031104. [38] Nakajima M, Sano H, Urabe I, Tagami J, Pashley DH. Bond
[15] Wang Y, Spencer P, Walker MP. Chemical profile of adhesive/ strengths of single-bottle dentin adhesives to caries-affected
caries-affected dentin interfaces using Raman microspectro- dentin. Oper Dent 2000;25:2—10.
scopy. J Biomed Mater Res A 2007;81(2):279—86. [39] Arrais CAG, Giannini M, Nakajima M, Tagami J. Effect of addi-
[16] Suga S, Soejima H, Tanaka Y. Electron probe X-ray tissues. J Dent tional and extended acid etching on bonding to caries-affected
Res 1967;46:1251—2. dentin. Eur J Oral Sci 2004;112:458—64.
[17] Takuma S, Ogiwara H, Suzuki H. Electron probe and electron [40] Erhardt MCG, Toledano M, Osorio R, Pimenta LA. Histomorpho-
microscope studies of carious dentinal lesions with reminera- logic characterization and bond strength evaluation of caries-
lized surface layer. Caries Res 1975;9:278—85. affected dentin/resin interfaces: effect of long-term water
[18] Tjäderhane L, Hietala E-L, Larmas M. Mineral element analysis exposure. Dent Mater 2008;24:786—98.
of carious and sound rat dentin by electron probe microanalyzer [41] Macedo GV, Yamauchi M, Bedran-Russo AK. Effect of chemical
combined with back-scattered electron image. J Dent Res cross-linkers on caries-affected dentin bonding. J Dent Res
1995;74:1770—4. 2009;88:1096—100.
[19] Daculsi G, Kerebel B, Le Cabellec M-T, Kerebel L-M. Qualitative [42] Erhardt MCG, Osorio R, Toledano M. Dentin treatment with
and quantitative data on arrested caries in dentin. Caries Res MMPs inhibitors does not alter bond strengths to caries-affected
1979;13:190—202. dentin. J Dent 2008;36:1068—73.
[20] LeGeros RZ, Tung MS. Chemical stability of carbonate- and [43] Wang Y, Spencer P. Analysis of acid-treated dentin smear debris
fluoride-containing apatites. Caries Res 1983;17:719—29. and smear layers using confocal Raman microspectroscopy. J
[21] LeGeros RZ, Sakae T, Bautista C, Retino M, LeGeros JP. Magne- Biomed Mater Res 2002;60:300—8.
sium and carbonate in enamel and synthetic apatites. Adv Dent [44] Lai SC, Mark YF, Cheung GS, Osorio R, Toledano M, Carvalho RM,
Res 1996;10:225—31. Tay FR, Pashley DH. Reversal of compromised bonding to oxi-
[22] Kuboki Y, Ohgushi K, Fusayama T. Collagen biochemistry of the dized etched dentin. J Dent Res 2001;80:1919—24.
two layers of carious dentin. J Dent Res 1977;56(10):1233—7. [45] Komori PCP, Pashley DH, Tjäderhane L, Breschi L, Mazzoni A, de
[23] Ohgushi K, Fusayama T. Electron microscope structure of the Goes MF, Wang L, Carrilho MR. Effect of 2% chlorhexidine
two layers of carious dentin. J Dent Res 1977;54:1019—26. digluconate on the bond strength to normal versus caries-
[24] Suppa P, Ruggeri Jr A, Tay FR, Prati C, BiasottoM, Falconi M, affected dentin. Oper Dent 2009;34:157—65.
Pashley DH, Breschi L. Reduced antigenicity of type I collagen and [46] Omar H, El-Badrawy E, El-Mowafy O, Atta O, Saleem B. Micro-
proteoglycans in sclerotic dentin. J Dent Res 2006;85:133—7. tensile bond strength of resin composite bonded to caries-
[25] Ogawa K, Yamashita Y, Ichijo T, Fusayama T. The ultrastructure affected dentin with three adhesives. Oper Dent 2007;32:24—
and hardness of the transparent layer of human carious dentin. J 30.
Dent Res 1983;62:7—10. [47] Nakajima M, Hosaka K, Yamauti M, Foxton RM, Tagami J.
[26] Daculsi G, Legeros RZ, Jean A, Kerebel B. Possible physico-chemi- Bonding durability of self-etching primer system to normal
cal processes in human dentin caries. J Dent Res 1987;66:1356—9. and caries-affected dentin under hydrostatic pulpal pressure
[27] Ito S, Saito T, Tay FR, Carvalho RM, Yoshiyama M, Pashley DH. in vitro. Am J Dent 2006;19:147—50.
Water content and apparent stiffness of non-caries versus [48] Pashley DH, Tay FR, Yiu C, Hashimoto M, Breschi L, Carvalho RM,
caries-affected human dentin. J Biomed Mater Res Part B Appl Ito S. Collagen degradation by host-derived enzymes during
Biomater 2005;72B:109—16. aging. J Dent Res 2004;83:216—21.
[28] Tagami J, Hosoda H, Burrow MF, Nakajima M. Effect of aging and [49] Tay FR, Pashley DH, Hiraishi N, Imazato S, Rueggeberg FA, Salz
caries on dentin permeability. Proc Finn Dent Soc 1992;88(Suppl. U, Zimmermann J, King NM. Tubular occlusion prevents water-
1):149—54. treeing and through-and through fluid movement in a single-
[29] Marshall GW, Habelitz S, Gallagher R, Balooch M, Balooch G, bottle, one-step self-etch adhesive model. J Dent Res 2005;84:
Marshall SJ. Nanomechanical properties of hydrated carious 891—6.
human dentin. J Dent Res 2001;80:1768—71. [50] Cehreli Z, Yazici AR, Akca T, Ozgunaltay G. A morphological and
[30] Zheng L, Hilton JF, Habelitz S, Marshall SJ, Marshall GW. Dentin micro-tensile bond strength evaluation of a single-bottle adhe-
caries activity status related to hardness elasticity. Eur J Oral sive to caries-affected human dentine after four different
Sci 2003;111:246—52. caires removal technique. J Dent 2003;31:429—35.
[31] Zheng L, Nakajima M, Higashi T, Foxton RM, Tagami J. Hardness [51] Sattabanasuk V, Burrow MF, Shimada Y, Tagami J. Resin adhesion
and Young’s modulus of transparent dentin associated with to caries-affected dentine after different removal methods.
aging and carious disease. Dent Mater J 2005;24:648—53. Aust Dent J 2006;51:162—9.