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Am J Dent. Author manuscript; available in PMC 2016 July 13.
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Published in final edited form as:

Am J Dent. 2015 December ; 28(6): 321–332.
Adhesive sealing of dentin surfaces in vitro: A review

Manar M Abu-Nawareg, BDS, MSc, PhD1,2, Ahmed Z Zidan, BDS, MSc, PhD3,4, Jianfeng
Zhou, DDS, PHD5, Kelli Agee, BS7, Ayaka Chiba, BDS6, Jungi Tagami, DDS, PhD6, and
David H Pashley, DMD, PhD7
1Department of Restorative Dentistry, Biomaterials Division, Faculty of Dentistry, King Abdulaziz
University, Jeddah, Saudi Arabia
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2Biomaterials Department, Faculty of Oral and Dental Medicine, Cairo University, Egypt
3Department of Restorative Dentistry, Biomaterials Division, Faculty of Dentistry, Umm Al-Qura
University, Mekkah, Saudi Arabia
4Biomaterials Department, Faculty of Dentistry, University of Modern Sciences and Arts, Egypt
5Department of Prosthodontics, Peking University School and Hospital of Stomatology, Beijing,
P.R. of China
6Department of Cariology and Operative Dentistry, Graduate School of Medical and Dental
Sciences, Tokyo Medical and Dental University, Tokyo, Japan
7Department of Oral Biology, Georgia Regents University, College of Dental Medicine, Augusta,
GA, USA
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Abstract
Purpose—The purpose of this review is to describe the evolution of the use of dental
adhesives to form a tight seal of freshly prepared dentin to protect the pulp from bacterial
products, during the time between crown preparation and final cementum of full crowns. The
evolution of these “immediate dentin sealants” follows the evolution of dental adhesives, in
general. That is, they began with multiple-step, etch-and-rinse adhesives, and then switched to the
use of simplified adhesives.
Methods—Literature was reviewed for evidence that bacteria or bacterial products diffusing
across dentin can irritate pulpal tissues before and after smear layer removal. Smear layers can be
solubilized by plaque organisms within 7–10 days if they are directly exposed to oral fluids. It is
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a3M ESPE, St. Paul, MN, USA

bKerr, Orange, CA, USA
cKuraray America Inc., New York, NY, USA
ddG-C Corp., Tokyo, Japan
eIvoclar Vivadent, Schaan, Liechtenstein
CORRESPONDING AUTHOR: David H. Pashley, DMD, PhD, Department of Oral Biology, College of Dental Medicine, Georgia
Regents University, Augusta, GA, 30912, Tel: 706-721-2031; [email protected].
Disclosure Statement: Drs. Abu Nawareg, Zidan, Zhou, Chiba, Tagami and Pashley have no commercial interest in any of the
products used in this study.
None of the authors claim any conflict of interest.
Abu-Nawareg et al. Page 2
likely that smear layers covered by temporary restorations may last more than one month. As long
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as smear layers remain in place, they can partially seal dentin. Thus, many in vitro studies
evaluating the sealing ability of adhesive resins use smear layer-covered dentin as a reference
condition. Surprisingly, many adhesives do not seal dentin as well as do smear layers.
Results—Both in vitro and in vivo studies show that resin-covered dentin allows dentinal fluid
to cross polymerized resins. The use of simplified single bottle adhesives to seal dentin was a step
backwards. Currently, most authorities use either 3-step adhesives such as Scotchbond Multi-
Purposea or OptiBond FLb or two-step self-etching primer adhesives, such as Clearfil SEc, Unifil
Bondd or AdheSEe, respectfully.
Introduction
When indirect restorations are used to restore function, dentists must seal the exposed dentin
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with temporary materials during the interval required to fabricate and cement the final
restoration. Full crown preparations expose up to 1 cm2 of dentin that contains more than 3
million tubules/cm2.1 Such tubules represent millions of microscopic “pathways to the pulp”
because they all terminate in the tooth pulp. Both enamel and cementum are impermeable
and nerve-free. These peripheral seals have very low permeabilities. However, once these
surface sealing hard tissues are removed from dentin surfaces, the exposed dentin becomes
highly permeable and very sensitive to hydrodynamic stimuli2. Because dentinal tubules
contain collagen fibrils/fibers, constrictions etc. their functional diameter (0.1 µm) is far
smaller than their 1.0 µm anatomical diameter3. This allows dentin to function like a 0.1 µm
Millipore filter to prevent bacteria from invading the pulp via dentinal tubules. However,
soluble bacterial products can permeate through dentin to the pulp where they provoke
immunological reactions and pulpal inflammation that threaten pulpal health4–6.
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Prevention of pulpal inflammation

Current prosthodontists recommend conservative tooth preparations using copious air-water
spray and intermittent cutting. This is followed by temporizing the preparations using a
variety of temporary filling materials and crown formers as long as there are no pre-existing
signs of pulp pathology. The rationale is that a healthy pulpodentin complex reacts to tooth
preparation by the deposition of tertiary dentin under those tubules that were cut during
cavity preparation that should wall off the prepared dentin and prevent bacterial invasion7.
On the other hand, old teeth have smaller pulps with fewer mesenchymal cells, and a poorer
blood supply8. Tertiary dentin requires more than 30 days to begin to form and that dentin
will not form if the pulp under the cut tubules produces an inflammatory response7. Old
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pulps contain pulp stones that interfere with endodontic treatment. If a temporary crown is
lost and the cut dentin is exposed, bacterial products will begin to diffuse down the tubules
toward the pulp. Pulpal cells will react to these bacterial antigens as if actual bacteria were
invading the pulp. This will trigger neurogenic inflammation in the pulp leading to pulpal
symptoms9,10.
Those that advocate immediate dentin sealing (IDS) of freshly prepared dentin seek to
protect the pulp from bacteria and bacterial products, using adhesive resins11–24. These

resins should prevent dentinal fluid from permeating from inside dentin, through
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polymerized resin to the surface. The resins should also prevent the inward diffusion of
bacterial products through the polymerized resin. This involves acid-etching dentin with
37% phosphoric acid for 15 sec when using etch-and-rinse adhesives. When using self-
etching adhesives, the two-bottle primer adhesives are preferred over single-bottle systems
because the acidic primer is covered with a solvent-free adhesive, rich in dimethacrylates
that create stronger resin films than monomethacrylates. Thicker resin seals are better than
thinner coatings, because they are less likely to be lacerated by multiple setting of crowns
during their final adjustments.
Combinations of resin adhesives covered by flowable composites provide tougher IDS than
resin films alone. Optibond FLb is an example of a 3-step, etch-and-rinse adhesive that uses
an adhesive that contains 48% fumed SiO2 and barium aluminoborosilicate Na2SiF625.
Scotchbond Multi-Purposea adhesive contains few fillers and is often covered with a
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flowable composite to make the IDS stronger. The final adhesive material is covered with
glycerin gel before polymerization to prevent the formation of an oxygen-inhibited layer.
Such a layer of unpolymerized comonomers interferes with polymerization of impression
material26.
Advantages of IDS include eliminating post-cementation sensitivity27, eliminating the

potential risk of bacterial leakage and pulpal irritation. Local anesthesia is often not required
for try-ins and occlusal adjustments. IDS should be considered for any patients at increased
risk of pulpitis due to immunosuppression, aged pulps, previous history of tooth sensitivity,
patients taking bisphosphonates, etc. who are at risk of developing bisphosphonate-induced
osteonecrosis of the jaw28. If such patients require root canal therapy and the roots are
perforated during RCT, such extraction sites fail to heal properly. Abutment teeth in such
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patients should receive IDS as a precautionary measure.
The influence of the thickness of IDS materials has also been reported29. That group found
that thicker adhesives increased fracture resistance of IDS Empress 2 ceramic crowns.
The purpose of this review was to follow the evolution of the use of dental adhesives to
create an immediate dentin seal to protect the pulpodentin complex from inflammatory
insults, in vitro. This review will begin with etch-and-rinse adhesives, followed by self-
etching primer/adhesives and finally single-bottle, simplified self-etching adhesives.
Historical review
The work of Bergenholtz4,5 showed that bacterial products could diffuse across freshly
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prepared dentin to induce pulpal inflammation. This lead Pashley et al. in 1992 to propose
sealing freshly prepared dentin with adhesive resins11. This was endorsed by Davidson’s
group in 199612, Paul and Schaerer 199713, and Özturk et al.14. Prof. Tagami advocated
“resin coating” of freshly cut dentin to prevent pulpal irritation15–17, and to increase
adhesion to dentin. Others have also stressed the importance of resin sealing18–24. In their
bKerr, Orange, CA, USA

a3M ESPE, St. Paul, MN, USA

1992 paper, Pashley et al.,11, the authors mounted the crowns of extracted human third
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molars on plexiglass blocks and prepared full crown preparations (Fig. 1). They measured
dentin permeability as a hydraulic conductance before and after sealing the preparations
with Prisma Univeral Bond 2f, Scotchbond 2a, Superbond C&Bg, Amalgambondh, Gluma
Bondi or Clearfil Photobondc. All adhesives reduced dentin permeability in vitro by at least
50%, with Prisma Universal Bond 2f sealing the best followed by Superbond C&Bg,
Amalgambondh and Scotchbond 2a. The worst seals were produced by Gluma Bondi. Bonds
made with Scotchbond 2a and Clearfil Photobondc gave excellent initial seals, but began to
leak after thermocycling the bonded dentin.
Bouillaguet et al.20 used extracted human third molar crowns flattened on the occlusal
surface and glued to a plexiglass base penetrated by 18 ga. stainless steel tubing to permit
measurement of dentin permeability. They measured the hydraulic conductance of acid-
etched dentin before and after bonding with Scotchbond Multi-Purposea, Prime & Bond 2.0f
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or All-Bond 2j (Table 1). All of these etch-and-rinse adhesives reduced dentin permeability
by 83%, 90% or 96.6%, respectively. Unfortunately, the authors only measured the initial
reduction in permeability. When Gregorie et al.30 evaluated the sealing ability of Optibond
Solo Plusb, Single Bonda, Excitee and Prime & Bond NTf, all these etch-and-rinse adhesives
only reduced dentin permeability to a residual value of 40%, while the self-etching
adhesives Clearfil SE Bondc, and Prompt-L Popa only reduced dentin permeability down to
a residual value of 36 and 16%, respectively (Table 2). They also only measured initial
permeability. Better initial permeability results were reported when Vaysman et al.31 using
Clearfil SE Bondc and Optibond Solo Plusf to seal acid-etched dentin. Both adhesives sealed
dentin 80–95%. All of the above authors remarked that no dental adhesive reduced dentin
permeability 100%.
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Elgalaid et al.32 were the third group to attempt to seal full crown preparations with Prime &
Bond NTf or leave them covered with a smear layer as controls. They were surprised to
discover that smear layers sealed dentin as well as the adhesive, but that either approach only
reduced dentin permeability by 55–64% for up to 3 weeks (the longest time studied).
Unfortunately, smear layers are very acid-labile and can solubilize in as little as one week
when exposed33. Carrilho et al.34 repeated Elgalaid’s32 work in 2007, and obtained similar
in vitro results. That is, smear layer/smear plugs seal dentin better than adhesive resins/resin
tags.
Water movement across resins, in vivo

Unfortunately, few clinical studies of “immediate dentin sealing” have been reported. Hu
and Zhu18 reported that the incidence of post-cementation hypersensitivity was significantly
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lower in teeth that received immediate dentin sealing with Prime & Bond NTf compared to
fDentsply, York, PA, USA

gSun Medical Co. Ltd., Shiga, Japan
hParkell, Edgewood, NY, USA
iHeraeus Kulzer, Hanau, Germany
cKuraray America Inc., New York, NY, USA
jBisco, Inc., Schaumberg, IL, USA
eIvoclar Vivadent, Schaan, Liechtenstein

abutment teeth that were prepared and temporized without immediate dentin sealing. Tay35
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and others have prepared human teeth for full crowns and then taken polyvinyl siloxane
impressions of smear layer-covered dentin (controls) or adhesive-coated dentin.
These impressions were poured up in epoxy resin for SEM examination of in vivo fluid
transudation across dentin “sealed” with smear layers or adhesives, as evidenced by the
presence of tiny bubbles of dentinal fluid on smear layer-covered or “adhesive-sealed”
dentin (Fig. 2). All two-step, self-priming, total-etch adhesives tested (Single Bonda, Prime
& Bond NTf, One-Stepj, Excite DSCe) were covered with fluid droplets indicating that
dentinal fluid had transudated across the polymerized adhesives in the 3–4 min required for
self-polymerization of the polyvinyl siloxane impression material. Less fluid droplets came
across smear-layer covered dentin than across polymerized resins.
Chersoni et al.36 extended the in vivo work of Tay et al.35 by making replicas of resin-
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covered dentin in vivo and also conducting fluid filtration studies across crown segments in
vitro (Fig. 3). When self-etch adhesives Adper Prompta, Xeno IIIf, iBondi and One-Up Bond
Fk were used to seal dentin, Adper Prompta and Xeno IIIf could not seal dentin as well as
did smear layer-covered dentin (Table 3). One-Up Bond Fk sealed dentin as well as did
smear layers. When the two-step self-etching system Unifil Bondd was used to seal dentin, it
reduced dentin permeability to 2.1% of smear layer covered dentin values (Table 3)! This
was due to the fact that the acidic primer layer was covered by a solvent-free hydrophobic
layer (Fig. 3). Unifil Bondd produced the best seal of dentin, in part, because it was a self-
etching system, and because it was covered with a neat hydrophobic resin that absorbed little
water30.
Clearly, not all polymerized resins should be used for immediate dentin sealing, for if
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dentinal fluid can transudate across the “resin-sealed dentin,” those water droplets might
interfere with polymerization of impression materials. Ghiggi et al.37 sealed dentin with
Clearfil SE Bondc (CSE) alone or CSE covered with a glycerin jelly to exclude oxygen and
polymerized through jelly. Other specimens were treated with CSE that was polymerized in
air, but the oxygen-inhibited layer was removed with alcohol, or the CSE was covered with
Protect Liner Fc (PLF), a flowable composite alone or the flowable was covered with a
glycerin jelly or the polymerized PLF was scrubbed with alcohol before taking impressions
with Express XTa or Impreguma. Their results showed that small amounts of impression
material remained attached to dentin sealed with CSE alone or PLF, but were not found on
CSE covered with jelly or scrubbed with alcohol. Magne and Nielsen24 reported that only
CSE used with Extrudeb generated ideal impressions. They did not recommend Impreguma
for taking impressions of immediate dentin seals.
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Immediate dentin seals, if treated properly, can serve as a foundation for indirect composite
inlays. Duarte et al.38 found that immediate dentin sealing with Adper Single Bonda gave
microtensile bond strengths of 51.1 MPa, while Adper Prompt L-Popa only gave 1.7 MPa
bond strength. If dentin is temporized without immediate dentin sealing, the subsequent use
kTokuyama Corp., Tokyo, Japan

ddG-C Corp., Tokyo, Japan

of Optibond FLb or CSEc for indirect restorations falls 11.6 MPa or 1.81 MPa,
respectively39. When those same adhesives were used for immediate dentin sealing and the
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final restoration delayed 1–12 weeks, the microtensile bond strengths exceeded 45 MPa for
both adhesives39. Dillenburg et al.40 reported that immediate dentin seals should be cleaned
of temporary cement with aluminum oxide powder and 37% phosphoric acid treatment,
followed by a second layer of the same adhesive. These microtensile bond strengths were
similar to the controls that were never temporized.
Water movement across polymerized resins, in vitro

Özok et al.41 prepared class II cavities (Fig. 4) in crown segments in vitro, and measured the
permeability of smear layer-covered dentin. Then the cavities were bonded with Scotchbond
1a or Prompt L-Popa following the manufacturer’s instructions, under 15 cm H2O of pulpal
pressure or 0 cm H2O pulpal pressure. Scotchbond 1a reduced dentin permeability 48%
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when bonded under 15 cm H2O pressure, but 88% when no pressure was applied (Table 4).
In contrast, Prompt L-Popa reduced dentin permeability 88% when 15 cm H2O was applied
during bonding, but 95% when no pulpal pressure was applied.
Itthagarun et al.42 created exposed, flat dentin surfaces in human dentin and then bonded
them with Prompt-L-Popa, Etch & Prime 3.0m, One-Up Bond Fk, Reactmer Bondl or Unifil
Bondd. Unifil Bondd lowered dentin permeability 98% to a residual post-bonded
permeability of only 2% of smear layer values (similar to the results of Chersoni et al.36
above), while Prompt L-Popa and Etch & Prime 3.0m didn’t seal dentin any better than did
the smear layer (Table 5). One-Up Bond Fk and Reactmer Bondl were better than Prompt L-
Popa and Etch & Primem but not as good as Unifil Bondd (Table 5).
Magne23 recommended the etch-and-rinse adhesive, OptiBond FLb, to seal dentin. After
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acid-etching and priming of dentin, the final adhesive layer is solvent-free and relatively
hydrophobic, like the adhesive of Unifil Bondd and creates an excellent seal. Indeed,
Scotchbond Multi-Purpose’sa adhesive produces good dentin sealing because it is also
solvent-free. Clearfil SE Bondc adhesive is another example of a solvent-free, relatively
hydrophobic resin blend that seals dentin well.
Grégorie et al.43 bonded smear layer-covered dentin in vitro with ten self-etching adhesives.
Smear layers reduced dentin permeability 40–50% compared to acid-etched values.
However, when they bonded the 4000 grit SiC smear layers with Xeno IIIf, AdhSEe, Adper
Prompt L-Popa, Etch & Primem or One-Up Bond Fk, the post-adhesion permeability fell 50–
60% compared to the initial acid-etched value (Table 6). Optibond Solo Plusb, Prime &
Bond NTf-treated dentin reduced dentin permeability 45.6 to 42.3%. Prime & Bondf non-
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rinse conditioner and 1 layer of Prompt L-Popa only reduced dentin permeability 16%
(Table 6).
mDegussa AG, Hanau, Germany

lShofu Inc., Kyoto, Japan

Use of potassium oxalate to seal tubules with crystals

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Yiu et al.44 reported that the in vitro dentin permeability of smear layer-covered dentin
varied from 9–11% of acid-etched values. When acid-etched dentin was treated with
BisBlockj (2.8% oxalic acid), the permeability fell to between 9.4- 11.9% of acid-etched
values, much like the smear layer covered dentin (Table 7). When acid-etched dentin was
bonded with One-Stepj, Single Bonda, OptiBond Solo Plusb or Prime & Bond NTf, the
permeability only fell to 31–34% of acid-etched values that were all significantly higher than
the smear layer or BisBlockj values (Table 7). However, when BisBlockj was used to
pretreat dentin prior to bonding with One-Stepj or Single Bonda, the dentin permeability fell
to values that were only 2 or 6%, respectively, far lower permeability values than were
produced by smear layers or by BisBlockj alone, indicating that a double seal by calcium
oxalate crystals and resin tags lowers dentin permeability. One-Stepj and Single Bonda
reduced dentin permeability almost to zero. In contrast, when BisBlockj-treated dentin was
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bonded with OptiBond Solo Plusb or Prime & Bond NTf, the permeability of dentin only fell
to 27–28%, about like the use of these adhesives without BisBlockj (Table 7). Further
studies were done to try to determine why OptiBond Solo Plusb and Prime & Bondf were
not as effective as One Stepj and Single Bonda. Table 7 shows that the pH of OptiBond Solo
Plusb and Prime & Bond NTf were 2.8 and 2.7, respectively. Clearly, OptiBond Solo Plusb
and Prime and Bond NTf were more acidic than the other two adhesives. When the
adhesives were analyzed for ionic fluoride, One-Stepj and Single Bonda contained 70 and
130 ppm F-, while OptiBond Solo Plusb contained 4527 ppm F- and Prime & Bond NTf
contained 3641 ppm F- (Table 7). Further, TEM studies of ammoniacal silver nitrate
immersed specimens revealed the presence of globular deposits into dentinal tubules that
may be CaF2-phosphate complexes. These were not found in One-Stepj or Single Bonda
bonded specimens.
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When low viscosity polyvinyl siloxane impressions were made of the BisBlockj pretreated,
resin-bonded surfaces, epoxy resin replicas were made for SEM examination. Figure 5
shows only a few droplets of water on the surface of One-Stepj or Single Bonda bonded
dentin, but extensive amounts of water had filtered across the polymerized resin of Prime &
Bond NTf or Optibond Solo Plusb in the 3–4 min required for setting of the impression
material.
Clearly, low pH and high fluoride concentrations somehow interfere with the sealing
properties of OptiBond Solo Plusb and Prime & Bond NTf, but not with One Stepj or Single
Bonda. When less acidic, low fluoride adhesives are combined with pretreatment by oxalic
acid, one obtains double sealing of dentinal tubules45.
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Fluid movement across polymerized resins

Sauro et al.46 extended the work of Tay et al.35 and Chersoni et al.36 by quantitating the
number of water droplets on various adhesive resins bonded to dentin (Fig. 6), and to then
correlate it with actual fluid flow transudation across the bonded dentin using the hydraulic
conductance technique (Fig. 7). They published a highly significant positive linear

regression equation showing an R2 = 0.96 of the relationship between the number of fluid
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droplets on resin surfaces and the permeability of the adhesives (Fig. 7).
Two years later, Sauro et al.47 measured droplet formation by tandem confocal scanning
microscopy (TSM) dentin sealed with G-Bondd, DC-Bondc, Single Bonda, OptiBond FLb or
Filtek Siloranea. The best sealing was obtained using G-Bondd. This was the exact opposite
of their results obtained in 2007. The authors explain that the polymerized G-Bondd films
looked frothy, but did not allow much fluid transudation. OptiBond FLb sealed dentin gave
the next to the best seal. DC Bondc and Single Bonda gave the worst seals.
Grégorie et al.48 tested the moisture-sensitivity of Prompt L-Popa versus Scotchbond 1XTa
by measuring the ability of these resins to seal dentin compared to their acid-etched values.
Scotchbond 1XTa was more sensitive to overly dry dentin than was Prompt L-Popa.
Scotchbond 1XTa reduced dentin permeability by 55%, while Prompt L-Popa reduced it by
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62%, although these values were not significantly different. These relatively poor seals
suggest that the ability of adhesive resins to seal dentin had not improved much over the
2000–2009 period.
Use of resin-modified glass ionomers

Rusin et al.49 evaluated the resin-modified glass ionomer (Vitrebond Plusa) for its ability to
seal dentin, when applied to acid-etched or smear layer-covered dentin. When applied to
smear layers, Vitrebond Plusa reduced dentin permeability 98.9 ± 1.1%, because it was a
second layer on top of a smear layer that contained smear plugs in the tubules. This is the
best seal that we have seen published in the literature. When Vitrebond Plusa was placed on
acid-etched dentin it created a hybrid layer complete with resin tags (Fig. 8). The Vitremer
Plusa matrix separated from the filler particles creating Vitremer Plus matrix resin tags about
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2 µm long. Vitrebond Plusa reduced the permeability of acid-etched dentin by 87.7 ± 18.6%.
This means that some specimens produced perfect seals, while others only sealed dentin
69%.
Use of 2-bottle self-etching primer adhesives

Clearly, most resins do not seal dentin as well as do enamel or cementum. Two step, self-
etching adhesives tend to seal better than do etch-and-rinse adhesives because the mildly
(pH 2–2.4) acidic versions barely etch through smear layers (Fig. 9). As many smear plugs
are more than 2 µm long and are covered by 1 µm thick smear layers, the mild etching of
self-etching adhesives fails to remove the smear plugs, preventing dentinal fluid from
contaminating dentin surfaces44. Self-etching adhesives only contain 25–35% water, while
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etching dentin with phosphoric acid and rinsing with water, leaves demineralized dentin
floating in 70 vol% water41. Thus, it is easier to displace 25–35% water from thin hybrid
layers than trying to displace 70 vol% water using etch-and-rinse adhesives.
For some etch-and-rinse adhesives (One-Stepj and Single Bonda), surface water can be
controlled by applying oxalic acid to acid-etched dentin prior to bonding. Oxalates do not
work with more acidic, high fluoride-containing products like OptiBond Solob or Prime &
Bond NTf44.

The two-step self-etching primer/adhesives like Unifil Bondd, Clearfil SE Bondc or Clearfil
Protect SEc or AdheSEe, confine their water and acidic monomers to their primers and cover
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the primed dentin with solvent-free, relatively hydrophobic resins that seal dentin much
better than do simplified, single bottle adhesives (e.g. G-Bondi, iBondj, Xeno IIIf, etc.). If
we assume that higher resin-dentin bond strengths represent improved dentin sealing, then
there are several papers that show that multiple resin coats improve dentin bonding.
Attempts to seal dentin using multiple coatings of adhesives has resulted in mixed success.
Pashley et al.50 compared applications of one versus two coats of Prompt L-Popa. Using one
layer of adhesive, as recommended, produced microtensile bond strength of only 14.2 ± 7.2
MPa (n=24). Application of two layers produced a µTBS of 29.7 ± 5.7 (n=23, p<0.001).
Transmission electron microscopy of the bonded specimens revealed a thin layer of
polymerized resin on top of the hybrid layer. There was about 10–15 µm of oxygen-inhibited
adhesive on top of the 5–7 µm polymerized resin. This layer was responsible for the low
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bond strength of single layers of adhesives.
Use of multiple layers of resin

In 2004, Hashimoto et al.51 tested the effects of multiple applications of OptiBond Solo
Plusb or Single Bonda on both microtensile bond strength and silver nanoleakage. The
results showed a progressive increase in bond strength and decrease in nanoleakage with
each additional layer, up to 4 coats. Solvent evaporation after each coating increased the
thickness of the adhesive layer. This result was confirmed by Ito et al.52 using the single
bottle, self-etch adhesives Xeno IIIf or iBondi. The results are summarized in Table 8.
The results revealed that the bond strengths with Xeno IIIf increased with the number of
coatings, just as in the Hashimoto et al.51, but the bond strengths were significantly higher
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after each coating, if the layer was light-cured (Table 8). The reverse was true with iBondi.
Using iBondi, simply evaporating the solvent of each layer increased bond strengths faster
than if each layer was evaporated and light-cured. While the results were very interesting,
the technique requiring multiple solvent evaporations and multiple light-curing is so
laborious that most clinicians would not adopt it.
There was one final group in the Ito et al.52 study, where after application of the first layer of
self-etching adhesive, the “primed” dentin surface was covered with a layer of solvent-free
Scotchbond Multi-Purposea (SBMP) adhesive, which was then light-cured. In the group 1
specimens, where only the solvent in the first layer was evaporated, but not light-cured,
application of one layer of SBMPa and its light-curing gave a bond strength of 27.8 ± 5.9
MPa. In group 2, where the single layer of Xeno IIIf was both evaporated and light-cured
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prior to application of SBMPa, the bond strength increased 232% to 64.7 ± 21.2 MPa (Table
8, 1 + SBMP column). Using iBondi in groups 3 and 4, the bond strengths were above 55
MPs regardless of whether the single layer of iBondi was only evaporated or was evaporated
and light-cured prior to application of SBMPa adhesive. Silver nanoleakage studies showed
that self-etching single-bottle adhesives exhibit much more nanoleakage than does SBMPa
adhesive because self-etch adhesives contain residual water, while SBMPa adhesives are
water-free (Figs. 10A and 10B).

The results of the Ito et al.52 study clearly show the benefits of covering self-etching
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adhesives with solvent-free, dimethacrylate-rich adhesives. This concept was reinforced by

the paper by Brackett et al.53. In that paper, the microtensile bond strengths of three single-
bottle self-etching adhesives Prompt L-Popa, iBondi and Xeno IIIf were compared when
they were used according to the manufacturer’s instructions and light-cured, or when the
cured adhesive was covered with an additional layer of a solvent-free, neutral,
dimethacrylyte-rich adhesive. The results are shown in Table 9, confirming that the use of
solvent-free adhesives over simplified self-etch adhesives improves bond strengths.
The question of whether resin-dentin bond strengths can be increased using multiple layers
of resin, seems to have been answered in the affirmative. However, Reis et al.54 asked
whether the durability of one-step self-etching adhesives would be improved by double
application or by an extra layer of hydrophobic dentin. Both the double layer and the
hydrophobic layer either improved the immediate bond strength, or did not differ from the
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results obtained with the manufacturer’s directions (Table 10). Resin-dentin bond strengths
after 6 months of water storage were higher when the additional layer of hydrophobic resin
was used compared to the results obtained with the manufacturer’s directions. These results
should be repeated but measuring dentin permeability instead of bond strength, and extended
to 12 months of water storage. Reis et al.55 repeated their 2008 study54 in a clinical trial of
retention of resin composites bonded with the Clearfil S3c or iBondi using either the
manufacturer’s directions or an additional hydrophobic layer (in this study, the solvent-free
adhesive of Scotchbond Multi-Purposea Adhesive system) bonded to noncarious cervical
lesions for 18 months. The results showed higher 18-month retention rates for both
adhesives if they were covered with an extra layer of hydrophobic resin, especially iBondi
(p<0.05)55.
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Evaluation of sealing using silver nitrate

Another approach to evaluating the sealing ability of various adhesives to dentin is to
measure silver nanoleakage56. This is done by immersing resin-bonded dentin into 50 wt%
ammoniacal silver nitrate for 24 hrs, followed by rinsing off excess AgNO3 and exposing the
specimens to photodeveloper and/or bright light to reduce the silver ions to metallic silver
grains that cannot diffuse after reduction.
Silver nitrate uptake discloses the presence and distribution of water-filled channels within
the hybrid layer and overlying adhesive layer. Figure 11 shows two transmission electron
micrographs of resin-dentin bonds made with single-bottle, simplified self-etching adhesive.
These adhesives contain 25–35% water to ionize their acidic monomers. Although clinicians
attempt to evaporate the residual water in the adhesives prior to light-curing, 5–15 sec is
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insufficient to remove all water57. Some of that residual water resides in the small lateral
branches of dentinal tubules (Fig. 11, pointer) that are sometimes referred to as “water-
trees”58. Water-trees sometimes seem to originate from hybrid layers (often from one or two
dentinal tubules), that extend up into the overlying adhesive layer (Fig. 11). Water-trees are
seldom seen in dentin bonds made with 2-step self-etching adhesives like Clearfil SE Bondc
because the water in the acidic primer is sealed by the water-free hydrophobic adhesive like
Clearfil SE Bondc adhesive or Scotchbond Multi-Purposea adhesive50.

Role of matrix metalloproteinase enzymes in bond degradation

Author Manuscript
When using etch-and-rinse adhesives, the etchant is 37% phosphoric acid. This acid is
strong enough to solubilize and extract all extrafibrillar and intrafibrillar apatite crystallites
from the top 8–10 µm of acid-etched dentin. Since the mineral content of dentin is about 70
vol%, the removal of all mineral from the dentin matrix is replaced by 70% water60. It is
very difficult to replace 70% water with adhesive monomers in the 30–60 sec most clinicians
use to infiltrate adhesives into dentin. The result of incomplete resin-infiltration is
incomplete water removal. Silver ions saturate any residual water-filled spaces56,60,61.
During acid-etching, not only is the dentin matrix exposed, but the matrix metalloproteinases
(MMPs) bound to the matrix is are uncovered and activated by acid-etching62. MMPs slowly
degrade collagen by adding water across specific peptide bonds in collagen62. The more
residual water in resin-dentin bonds, the greater the rate of hydrolysis. Collagen degradation
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not only lowers resin-dentin bond strength, but slowly increases dentin permeability by
loosening resin tags and destroying the hybrid layer60. Thus, for many reasons, it is
important to minimize residual water in resin-dentin bonds.
One approach to minimizing residual water at bonded interfaces is to treat the 8–10 µm
demineralized layer with 10% NaOCl gel63. This treatment dissolved some of the collagen
fibrils in the hybrid layer and lowered the bond strength of Single Bonda by 69% and Prime
& Bond NTf by 69%63. Others have shown that a solution of 5% NaOCl is more effective
than gels. The use of 5% NaOCl as an endodontic irrigant to remove exposed collagen is
well known64. It is used, in part, to disinfect root canals of contaminating bacteria as well as
remove exposed collagen so that endodontic seals are placed on stiff mineralized dentin
rather than soft, demineralized dentin. Sodium hypochlorite has a pH of 12. It is a strong
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oxidizing agent. Its action lowers the bond strength of free-radical polymerizing resins. This
oxidized state can be reversed within 2–5 min by treating NaOCl-treated dentin with 10%
sodium ascorbate65,66. The only disadvantage is that a 3 GPa adhesive layer comes in direct
contact with 18 GPa underlying mineralized dentin, since most of the 8–10 µm thick
demineralized layer is removed by NaOCl.
Are extra steps of pretreatment able to improve resin sealing of dentin as was seen in the Yiu
et al.44 study with oxalate? Oxalates can be used with some etch-and-rinse adhesives but not
with others.
Multi-step approach to sealing dentin

Abu-Nawareg67 compared the dentin sealing ability of three adhesive systems: Adper Single
Author Manuscript
Bond Plusa, AdheSEe, and G-Bondd representing an etch-and-rinse adhesive, a two-step

self-etching primer adhesive, and a single bottle, simplified self-etching adhesive.
Single Bond Plusa controls (no pretreatments) showed the highest residual permeabilities,
25.3 ± 0.7% at day 1 and 40.4 ± 1.4% (p<0.05) after 2 months in a simulated body fluid at
37°C. When Single Bond Plusa specimens were pretreated with oxalate (BisBlockj) just
before bonding, their 1 day permeabilities were only 11.7 ± 0.8% and their 2 month values
were 17.4 ± 0.8% (p<0.05). Sequential pretreatment of etched dentin with both NaOCl and

oxalate produced a significant (p<0.05) further reduction in residual permeability to 5.7

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± 0.6 and 7.6 ± 0.5% after 1 day or 2 months, respectively (Fig. 12).
Control specimens bonded with AdheSEe showed the greatest sealing of dentin by
exhibiting residual post-bonded permeabilities of only 11.0 ± 0.6 and 15.1 ± 0.7% after 1
day or 2 months, respectively (Fig. 12). When AdheSEe bonded specimens were pretreated
with oxalate (BisBlockj), their dentin permeability fell (p<0.05) to 2.6 ± 0.6 and 5.0 ± 0.4%
after 1 day or 2 months storage, respectively. Sequential pretreatment of dentin with NaOCl,
plus oxalate produced the lowest permeability recorded in that study, 0.80 ± 0.2 and 1.2
± 0.4%, respectively, after 1 day or 2 months.
Control specimens bonded with G-Bondd produced intermediate residual permeabilities of

16.2 ± 0.8 and 20.5 ± 0.7% after 1 day or 2 months, respectively. Oxalate pretreated
specimens bonded with G-Bondd showed significantly (p<0.05) higher permeabilities 22.1
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± 0.9 (day 1) versus 30.8 ± 0.8% (60 days), respectively (Fig. 12). When G-Bondedd
specimens were subsequently pretreated with NaOCl and oxalate, their permeabilities were
significantly higher from the oxalate alone values (Fig. 12).
The superior sealing ability of AdheSEe, a two-bottle, self-etching primer adhesive, mimics
the excellent results obtained by others36,37 using Unifil Bondd. In such two bottle systems,
the water-containing acidic primer is scrubbed on the dentin for 20 sec, dried, and then
covered with a water-free, dimethacrylate-containing adhesive that provides an excellent
seal. Other two-bottle self-etching adhesives such as Clearfil SE Bondc or Clearfil Protect
SEc or Optibond Solob should work equally well.
The use of Adper Prompt L-Popa for dentin sealing of crown preparations is not
recommended because it etches far more deeply and removes smear plugs as well as smear
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layers, allowing dentinal fluid access to the bonded interface. As the depth of etch is nearly
as deep as that produced by 37% phosphoric acid, there is concern that adhesive monomers
may not infiltrate to the full depth of the etch58, allowing dentin proteases to degrade the
resin-dentin bond62.
Recent expanded applications of resin sealing of dentin

In the U.S., Pashley’s group began sealing the coronal top of root canal fillings with unfilled
adhesives so that the pink gutta percha could be visualized through an adhesive intracoronal
seal68 in case the root canal filling needed to be removed sometime later. Others used
Vitrebonda, but it is not transparent70. Intracanal seals protect root canal fillings during the
time interval between completion of root canal treatment and permanent restoration of the
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tooth.
In Japan, Tagami’s group were also advocating intracoronal seals to prevent microleakage in
endodontically-treated teeth69,71. Imazato et al.72 recommended the use of antibacterial
monomers. Nikaido et al.73 reported that the bond strength of resin cements to resin-coated
dentin could be improved by covering the adhesive with a flowable composite. Magne’s
latest recommendations for “immediate dentin sealing” also recommend covering resin seals
with flowable composites74. To treat exposed root surfaces in elderly patients with cervical

caries, Daneshmehr et al.75 and Tajima et al.71 demonstrated that coating root surfaces with
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adhesive resins decreased biofilm adherence compared to untreated root surfaces. Others
have incorporated antimicrobial quaternary ammonium methacrylates like 12-
methacryloyloxydodecyl pyridinium bromide (MDPB) into adhesives72. The use of MDPB
is indicated when bonding to dentin containing bacteria72. More recently, MDPB has been
shown to be a potent inhibitor of dentin MMPs and cathepsin K77. Thus, resins can be
bioengineered to have therapeutic effects76. By increasing the concentration of acidic
monomers in adhesive blends, Brambilla et al.78 were able to inhibit S. mutans colonization.
Summary
The use of adhesive resins for immediate sealing of dentin (ISD) began in 1992, using early
generation dentin bonding agents alone. As bonding agents improved, in vitro studies
demonstrated that Scotchbond Multi-Purposea (SBMP) adhesive or Optibond FLb sealed
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dentin better than most other adhesives and so they were widely employed in ISD. When
self-etching adhesives were developed, the best dentin seals were produced by Unifil
Bondd36 or Clearfil SE Bondc24,37,39 (CSE). These adhesive systems seal the acid-etched
dentin with a solvent-free adhesive that is rich in dimethacrylates that have been shown to
minimize water sorption into the bonded assembly75,76. Others empirically found that
covering SBMPa or CSEc with a flowable composite such as Protect Liner Fc provides
additional sealing benefits24,37,38, while various pretreatments can improve resin sealing of
dentin67, though they require extra bonding steps. More clinical studies need to be done to
determine if IDS prevents later adverse pulpal responses to indirect restorative procedures.
Magne’s latest recommendations74 include the use of flowable composite over unfilled
adhesives as an alternative to the use of filled adhesives, and to cover the resin sealed
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preparation with glycerine gel to prevent forming a layer of oxygen inhibited resin at the
surface that interferes with polymerization of impression material. More controlled clinical
trials need to be done to statistically test whether post-restorative pulpal health is
significantly better in teeth protected by IDS, compared to the use of conventional
temporization.
Acknowledgments
This work was supported, in part, by grant R01 DE015306 from the NIDCR, a GRU/GT Seed Grant to DP (PI) and
by the Deanship of Scientific Research (DSR), King Abdulaziz University, under grant No. (1 - 165 - 35 - HiCi).
The authors, therefore, acknowledge technical and financial support of KAU. The authors are grateful to Mrs.
Michelle Barnes for her outstanding secretarial support.
This study was not supported by any manufacturer.

Author Manuscript
Dr. Abu-Nawareg is an Associate Professor of Restorative Dentistry and Biomaterials, Faculty of Dentistry, King
Abdulaziz University, Jeddah, Saudi Arabia and Faculty of Oral and Dental Medicine, Cairo University, Egypt; Dr.
Ahmed Zidan is an Assistant Professor of Restorative Dentistry and Biomaterials, Faculty of Dentistry, Umm Al-
Qura University, Mekkah, Saudi Arabia and Faculty of Dentistry, University of Modern Sciences and Arts, Egypt;
Dr. Jianfeng Zhou is a member of the Faculty of Dentistry, Peking University School and Hospital of Stomatology,
Beijing, P.R. of China; Dr. Akaya Chiba is a graduate student of Department of Cariology and Operative Dentistry,
Graduate School of Medical and Dental Sciences, Tokyo Medical and Dental University, Tokyo, Japan; Dr. Junji
Tagami is the Chairman of the Department of Cariology and Operative Dentistry, Graduate School of Medical and
Dental Sciences, Tokyo Medical and Dental University, Tokyo, Japan; Dr. David Pashley is an Emeritus Regents
Professor of Oral Biology, College of Dental Medicine, Georgia Regents University, Augusta, GA, USA.

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prepared teeth: An in vitro study. J Conserv Dent. 2009; 12:65–68. [PubMed: 20617069]
71. Tajima K, Nikaido T, Inoue G, Ikeda M, Tagami J. Effect of coating root dentin surfaces with
adhesive materials. Dent Mater J. 2009; 28:578–586. [PubMed: 19822989]
72. Imazato S, Torii Y, Takatsuka T, Inoue K, Ebi N, Ebisu S. Bactericidal effect of dentin primer
containing antibacterial monomer methacryloyloxydodecyl pyridinium bromide (MDPB) against
bacteria in human carious dentine. J Oral Rehabil. 2001; 28:314–319. [PubMed: 11350583]
73. Nikaido T, Cho E, Nakajima M, Tashiro H, Toba S, Burrow MF, Tagami J. Tensile bond strengths
of resin cements to bovine dentin using resin coating. Am J Dent. 2003; 16:A41–A46.
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74. Magne P. IDS:Immediate dentin sealing for tooth preparations. J Adhes Dent. 2014; 16:594.
[PubMed: 25564033]
75. Daneshmehr L, Matin K, Nikaido T, Tagami J. Effects of root dentin surface coating with all-in-
one adhesives materials on biofilm adherence. J Dent. 2008; 36:33–41. [PubMed: 18073132]
76. Imazato S, Ma S, Chen J-h, Xu HHK. Therapeutic polymers for dental adhesives: Loading resins
with bio-active components. Dent Mater. 2014; 30:97–104. [PubMed: 23899387]
77. Tezvergil-Mutluay A, Agee KA, Mazzoni A, Carvalho RM, Carrilho M, Tersariol IL, Nascimento
FD, Imazato S, Tjäderhane L, Breschi L, Tay FR, Pashley DH. Can quaternary ammonium
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25467953]
78. Brambilla E, Ionescu A, Mazzoni A, Cadenaro M, Gagliani M, Ferraroni M, Tay FR, Pashley DH,
Breschi L. Hydrophilicity of dentin bonding systems influences in vitro Streptococcus mutans
biofilm formation. Dent Mater. 2014; 30:926–935. [PubMed: 24954666]
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CLINICAL SIGNIFICANCE
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Although newly developed adhesive resins have attempted to improve dentin sealing,
many such attempts failed. The use of two-step self-etching primer adhesives that
combine the use of an acidic primer with a solvent-free adhesive layer give excellent
sealing in vitro. Alternatively, the use of three-step, etch-and-rinse adhesive systems like
Scotchbond Multi-Purposea or OptiBond FLb that also use solvent-free adhesives seal
dentin very well, in vitro.
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Fig. 1.
Schematic of the apparatus used to measure dentin permeability. N2 gas passed into a
pressure vessel containing a beaker of water. The water passes through the system at
whatever pressure is used. The rate of movement of a tiny air bubble in a 25 µL micropipette
quantitates how much water permeates across exposed dentin. The microsyringe adjusts the
position of the air bubble for the next trial (from Pashley et al.11, with permission).
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Fig. 2.
SEM micrographs of epoxy resin replicas of crown preparations taken in vivo. (A) Smear
layer(s) covered dentin showing how microdrops of dentinal fluid transudated across the
smear layer and were trapped by the impression material in the 2–3 min required for the
setting time. (B) Resin-covered crown preparation sealed with Single Bonda, a 2-step one-
bottle adhesive. Note the presence of extensive fluid mirodrops. (C) Higher magnification of
(B) showing the presence of nanodroplets of dentinal fluid. (D) Resin-coated dentin after
gentle clearing with pumice slurry. This produced cracks and partial removal of adhesive
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(arrow) exposing underlying dentin (from Tay et al.35, with permission).

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Fig. 3.
SEMs of resin replicas of crown preparations of vital teeth covered with (A) smear layer.
Note presence of a few microdroplets of transudated dentinal fluid trapped by the impression
material. (B) Unifil Bondd bonded surface after removal of O2-inhibited resin. No fluid
droplets were seen when using this two bottle, self-etching primer adhesive (from Chersoni
et al.36, with permission).
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Fig. 4.
Schematic of the apparatus used for measuring the dentin permeability of class V cavities
before and after restoration with bonded composites (from Özok et al.41, with permission).
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Fig. 5.
SEM micrograph of epoxy resin replicas taken from acid-etched dentin treated with 2.7%
potassium oxalate (pH 2.7) prior to bonding with adhesives. (A) One Stepj bonded dentin
with only a few microdrops of fluid transudation. (B) Single Bonda bonded dentin showed
few microdrops (pointer) and nanodrops (triangle). (C) Prime & Bond NTf bonded dentin
showed massive numbers of microdrops that had transudated across the polymerized
adhesives. (D) Optibond Solo Plusb bonded dentin contained so many microdroplets that
they coalesced into pools of fluid (from Yiu et al.44, with permission).
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Fig. 6.
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SEM microscopy impression replicas of bonded dentin before and 3 min after application of
a physiologic pulpal pressure (20 cm H2O). (A) Dentin bonded with One Up Bond F Plusk
with no pulpal pressure. (B) Same specimen after application of pulpal pressure. (C) Dentin
specimens bonded with Clearfil S3c with pressure. (D) Specimen bonded with G-Bondd with
pressure. (E) Dentin specimens bonded with Clearfil Protect Bondc, a two-bottle self-etching
adhesive where the primed dentin is covered by a solvent-free adhesive (from Sauro et al.46,

with permission). Abbreviations: CPB = Clearfil Protect Bondc; G = G-Bonda; CS3 =

3
Clearfil S -Bondc, OUB-F = One-Up Bond F Plusk.
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Fig. 7.
Regression analysis between adhesive permeability (abscissa) and number of microdroplets
of fluid on the bonded surface (ordinate) after application of 20 cm H2O pressure. A
significant (p<0.001) positive correlation (R2 = 0.96) was seen between the two variables
(from Sauro et al.46, with permission).
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Fig. 8.
SEM of Vitrebond Plusa light-cured glass ionomer liner/base applied to acid-etched dentin.
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Resin tags of the Vitrebonda matrix separated from the GIC fillers, extended 2 µm into open
tubules (from Rusin et al.49, with permission).
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Fig. 9.
Schematic illustrating the smear layer/smear plug complex on the left. When a weakly acidic
primer is applied, it loosens up the smear layer and the smear plug and infiltrates them with
resin (Violet). The presence of residual smear plugs prevents outward seepage of dentinal
fluid during bonding. After application of the water-free, neutral adhesive (purple), the bond
is well-sealed (from Pashley59, with permission).
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Fig. 10.
TEM micrographs of (A) dentin bonded with a coating of iBondi, followed by solvent
evaporation and light-curing. The bonded surface was then coated with Scotchbond Multi-
Purposea adhesive that was light-cured. After soaking in 50% ammoniacal silver nitrate
overnight, the specimens were processed for transmission electron microscopy (TEM). Note
the moderate silver nanoleakage in the bottom layer of iBondi adhesive (A) and the near
absence of nanoleakage in the SBMPa adhesive (R). (B) Dentin bonded with one layer of
Xeno IIIf, then the solvent was evaporated and the surface light-cured. The bonded surface
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was covered with one coat of water-free SBMPa adhesive (R). Note there is much less silver
nanoleakage in (R) than in (A) (from Ito et al.52, with permission).
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Fig. 11.
Transmission electron micrographs of dentin bonded with an all-in-one adhesive, incubated
in 37°C water for 24 h, followed by immersion in 50% ammoniacal silver nitrate overnight
to show the presence and distribution of residual water in hybrid layers (H) and adhesive
layer (A) by silver grains. Silver filled branching channels are called “water-trees”
(pointers). Spot-like silver deposits are simply called nanoleakage (from Pashley59, with
permission).
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Fig. 12.
Permeability of human dentin after bonding with Single Bonda, AdhSEe or G-Bondd using
the manufacturer’s instructions, or after pretreatment with 2.7% potassium oxalate (pH 2.7),
or after sequential pretreatment with 5.25% NaOCl followed by oxalate, after 1 day or 2
months (from Abu-Nawareg67, Adhesive sealing of dentin, Cairo University, PhD Thesis,
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2011, with permission).

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Table 1
Effects of bonding on the permeability of human dentin.

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Hydraulic conductance of dentin (µL min−1 cm−2 cm H2O−1)
Adhesive Smeared dentin Etched dentin Bonded dentin

Systems
SBMP Plusa b1.1 ± 0.7×10−2 (24.4%) a4.5 ± 3.0×10−2 (100%) b0.78 ± 0.6×10−2 (17%)
P&B 2.0f b1.0 ± 0.6×10−2 (20%) a5.0 ± 3.2×10−2 (100%) c0.5 ± 0.4×10−2 (10%)
All-Bond 2j b1.2 ± 1.0×10−2 (23%) a5.2 ± 3.9×10−2 (100%) c0.24 ± 0.1×10−2 (3.4%)
Values are mean hydraulic conductances ± SD (n=12). Values in parentheses are the hydraulic conductance expressed as a percent of the control,
acid-etched values that were defined as 100%. Groups identified by the same superscript are not significantly different (from Bouillaguet et al.20,
with permission).
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Table 2
Ability of various adhesives to seal dentin.

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Bonding agent Acid-etch permeability Residual permeability

after bonding
Excitee 150.13 ± 56.26a 40.21 ± 23.09a
Optibond Solo Plusb 175.77 ± 30.19a 38.53 ± 21.87a
Single Bonda 138.30 ± 27.08a 42.79 ± 13.61a
Prime & Bond NTf 137.82 ± 36.32a 41.87 ± 14.926a
Clearfil SE Bondc -- 36.42 ± 20.30ab
Prompt L-Popa -- 16.24 ± 15.66b
Values expressed in percentage decrease (−) or increase (+) with respect to baseline value (n=6). Mean ± SD, Duncan’s test (different superscript
letters, a, b, or ab, indicate different groups (from Grégorie et al.30, with permission).
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Table 3
Fluid conductance across dentin before and after bonding.

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% Fluid flow compared to acid-etched controls
Adhesives self-etch Smear layer covered Bonded dentin
Adper Prompta 17.3 ± 4.5A 28.3 ± 4.4A
Xeno IIIf 12.4 ± 6.2A 24.2 ± 2.9A,B
iBondi 15.1 ± 5.6A 18.7 ± 3.3B
One-Up Bond Fk 14.0 ± 3.1A 14.9 ± 5.0B
Two-step
Unifil Bondd 18.2 ± 5.0A 2.1 ± 2.1C
Groups identified by different superscript letters are significantly different (p<0.05) (from Chersoni et al.36, with permission).
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Table 4
Percent reduction in dentin permeability in class V composite restorations bonded with Scotchbond or Prompt
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L-Pop with or without pulpal pressure (15 cm H2O).
Percent reduction in permeability
Adhesive with pulp pressure without pulpal pressure
Scotchbond-1a 48.2 ± 49.2a 88.3 ± 19.1b
Prompt L-Popa 88.4 ± 17.3b 94.6 ± 7.8b
Groups identified by different superscript letters were significantly different (p<0.05) (from Özok et al.41, with permission).
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Table 5
Fluid flow across bonded dentin as a percent of maximum acid-etched values.

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Fluid flow (% of maximum) measured
Adhesives across smear layers across bonded dentin
Single-step
Prompt L-Popa 18.9 ± 5.3A 19.2 ± 3.6A
Etch & Prime 3.0m 18.9 ± 4.4A 17.4 ± 5.8A,B
One-Up Bond Fk 14.8 ± 4.4A 7.7 ± 4.9C
Reactmer Bondl 13.1 ± 3.9A 8.9 ± 5.7B,C
Two-step
Unifil Bondd 18.2 ± 5.0A 2.1 ± 2.1D
Groups identified by different superscript letters are significantly different (p<0.05) (from Itthagarun et al.42, with permission).
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Table 6
Dentin permeability of specimens after bonding with self-etching adhesives, compared to acid-etched controls.
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Adhesives Reductions in permeability after bonding
Xeno IIIf −68.9 ± 15.7%a
AdhSEe −58.2 ± 26.8%a,b
Adper Prompt L-Popa −51.0 ± 33.2%a,b
Etch & Prime 3.0m −56.8 ± 26.3%a,b
One-Up Bondk −60.5 ± 27.3%a,b
Optibond Solo Plus SEb −45.6 ± 34.4%a,b
Prime & Bond NT controlf −42.3 ± 5.1%b
Clearfil SE Bondc −35.5 ± 14.7%b,c
Prime & Bond NRC NTf −16.4 ± 33.3%c

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Prompt L-Popa −16.3 ± 13.3%c
Values are mean ± SE, N=10. Groups identified by different superscript letters are significantly different (p<0.05). Smear layer was created using
4000 grit SiC paper. Only 1 layer of adhesive was used with Prompt L-Pop, while multiple layers were used with Adper Prompt L-Pop. Prime &
Bond NRC NT is a no rinse conditioner that does not require water rinsing, used with Prime & Bond NT adhesive (from Gregorié et al.43, with
permission).
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Table 7
Effects of adhesives on fluid conductance of dentin.
Percent of fluid flow at 20 cm H2O pressure
Adhesive Smear layer Oxalate Tx Oxalate Tx Adhesive pH F− ppm

covered only plus adhesive only
Abu-Nawareg et al.
One Stepj 11.1 ± 2.0b 9.4 ± 1.9b 2.0 ± 0.9a 33.6 ± 8.9c 4.6 70
Single Bonda 10.8 ± 1.8b 9.9 ± 2.5b 6.0 ± 1.7a,b 34.2 ± 11.3c 3.6 130
OptiBond Solo Plusb 10.7 ± 5.9b 11.9 ± 5.6b 28.3 ± 12.2c 31.4 ± 4.7c 2.8 4527
Prime & Bond NTf 8.7 ± 1.7b 10.9 ± 4.7b 27.5 ± 10.8c 31.1 ± 6.3c 2.7 3641
Fluid flow from acid-etched dentin was assigned a value of 100%. Each tooth served as its own control. Groups identified by different superscript letters are significantly different (p<0.05) (from Yiu et
al.44, with permission).

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Table 8
Effects of multiple layers of two self-etch adhesives on microtensile bond strength.
Layers
Groups 1 2 3 4 5 1 + SBMP
Xeno IIIf 7.2 ± 6.3a 22.6 ± 9.2a,b 30.0 ± 9.9b 43.5 ± 7.7c 41.4 ± 8.0c 27.8 ± 5.9b
Abu-Nawareg et al.
(evaporation)
Xeno IIIf 7.2 ± 6.3a 47.3 ± 19.2b 65.4 ± 20.4d 81.8 ± 20.8d 68.9 ± 22.6d 64.7 ± 21.2d
(evaporation
+ 1c)
iBondi 12.2 ± 7.5A 18.5 ± 6.2A 30.6 ± 7.0B 34.2 ± 6.0B,C 51.6 ± 14.8B,C 62.3 ± 23.0C
(evaporation)
iBondi 12.2 ± 7.1A 39.6 ± 15.2B 42.7 ± 12.3B,C 36.6 ± 7.7B 35.8 ± 13.4B 58.0 ± 23.5C
(evaporation
+ 1c)
Values are mean ± SD in MPa, N=16. Groups identified horizontally by different superscript letters are significantly different (p<0.05) (from Ito et al.52, with permission). +lc = with light-curing of each
layer.

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Table 9
Microtensile bond strengths of dentin specimens bonded with simplified, all-in-one adhesives alone, or plus an
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additional layer of hydrophobic resin from the same manufacturer.
Adhesive Microtensile bond strength (MPa)
iBondi 41.0 ± 17.7a
iBond + Gluma Solid Bond Si 53.5 ± 19.0b
Prompt L-Popa 16.4 ± 9.9c
Prompt L-Pop + Scotchbond Multi-Purpose adhesivea 56.4 ± 21.8b
Xeno IIIf 10.3 ± 8.3c
Xeno III + experimental adhesivef 25.8 ± 8.0c
Values are mean ± SD, N=5. Groups identified by different superscript letters are significantly different (p<0.05) (from Brackett et al.53, with
permission).
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Table 10
Microtensile bond strength of self-etching adhesives to dentin measured immediately or after 6 months, using
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manufacturer’s instructions or double application or an extra layer of hydrophobic resin.*
Microtensile bond strength to dentin
Adhesive Time Manufacturer Double Hydrophobic layer

Directions application
Prompt L-Popa Immediately 24.3 ± 3.1b 45.3 ± 6.4a 29.5 ± 4.9b
6 month 16.9 ± 4.1c 17.2 ± 4.6b 29.1 ± 3.6b
Xeno IIIf Immediately 30.0 ± 1.2a 33.8 ± 3.4b 49.8 ± 3.7a
6 month 25.2 ± 3.9b 30.3 ± 4.2b 43.2 ± 4.8a
iBondi Immediately 19.1 ± 2.4b 29.2 ± 2.2a 37.6 ± 3.4a,b

6 month 18.1 ± 4.8b 26.4 ± 3.9b 28.2 ± 3.1b
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Values are means ± SD, in MPa.

*
Hydrophobic layer was the adhesive from Clearfil SE Bondc. Groups identified by different superscript letters are significantly different at p<0.05
(from Reis et al.54, with permission).
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Published in final edited form as:

Adhesive sealing of dentin surfaces in vitro: A review

a3M ESPE, St. Paul, MN, USA

Prevention of pulpal inflammation

Am J Dent. Author manuscript; available in PMC 2016 July 13.

Advantages of IDS include eliminating post-cementation sensitivity27, eliminating the

patients should receive IDS as a precautionary measure.

bKerr, Orange, CA, USA

Am J Dent. Author manuscript; available in PMC 2016 July 13.

Water movement across resins, in vivo

fDentsply, York, PA, USA

Am J Dent. Author manuscript; available in PMC 2016 July 13.

kTokuyama Corp., Tokyo, Japan

Am J Dent. Author manuscript; available in PMC 2016 July 13.

Water movement across polymerized resins, in vitro

mDegussa AG, Hanau, Germany

Am J Dent. Author manuscript; available in PMC 2016 July 13.

Use of potassium oxalate to seal tubules with crystals

Fluid movement across polymerized resins

Am J Dent. Author manuscript; available in PMC 2016 July 13.

Use of resin-modified glass ionomers

Use of 2-bottle self-etching primer adhesives

Am J Dent. Author manuscript; available in PMC 2016 July 13.

bond strength of single layers of adhesives.

Use of multiple layers of resin

Am J Dent. Author manuscript; available in PMC 2016 July 13.

adhesives with solvent-free, dimethacrylate-rich adhesives. This concept was reinforced by

Evaluation of sealing using silver nitrate

Am J Dent. Author manuscript; available in PMC 2016 July 13.

Role of matrix metalloproteinase enzymes in bond degradation

Multi-step approach to sealing dentin

Bond Plusa, AdheSEe, and G-Bondd representing an etch-and-rinse adhesive, a two-step

Am J Dent. Author manuscript; available in PMC 2016 July 13.

oxalate produced a significant (p<0.05) further reduction in residual permeability to 5.7

Control specimens bonded with G-Bondd produced intermediate residual permeabilities of

Recent expanded applications of resin sealing of dentin

Am J Dent. Author manuscript; available in PMC 2016 July 13.

This study was not supported by any manufacturer.

Am J Dent. Author manuscript; available in PMC 2016 July 13.

mechanical preparation for veneering. Am J Dent. 1996; 9:57–60. [PubMed: 9522686]

hypersensitivity. Int J Prosthodont. 2010; 23:49–52. [PubMed: 20234892]

Am J Dent. Author manuscript; available in PMC 2016 July 13.

Prosthet Dent. 2007; 98:166–174. [PubMed: 17854617]

Am J Dent. Author manuscript; available in PMC 2016 July 13.

Am J Dent. Author manuscript; available in PMC 2016 July 13.

durability: Control of collagen degradation by matrix metalloproteinase and cysteine cathepsins.

Am J Dent. Author manuscript; available in PMC 2016 July 13.

Am J Dent. Author manuscript; available in PMC 2016 July 13.

Am J Dent. Author manuscript; available in PMC 2016 July 13.

(arrow) exposing underlying dentin (from Tay et al.35, with permission).

Am J Dent. Author manuscript; available in PMC 2016 July 13.

Am J Dent. Author manuscript; available in PMC 2016 July 13.

Am J Dent. Author manuscript; available in PMC 2016 July 13.

Am J Dent. Author manuscript; available in PMC 2016 July 13.

Am J Dent. Author manuscript; available in PMC 2016 July 13.

with permission). Abbreviations: CPB = Clearfil Protect Bondc; G = G-Bonda; CS3 =

Am J Dent. Author manuscript; available in PMC 2016 July 13.