Journal of Dentistry (2004) 32, 611621

www.intl.elsevierhealth.com/journals/jden

Single-bottle adhesives behave as permeable

membranes after polymerization.
I. In vivo evidence
F.R. Taya,*, R. Frankenbergerb, I. Krejcic, S. Bouillaguetc,
D.H. Pashleyd, R.M. Carvalhoe, C.N.S. Laia
a
Faculty of Dentistry, Pediatric Dentistry and Orthodontics, University of Hong Kong,
34 Hospital Road, Hong Kong
b
Policlinic for Operative Dentistry and Periodontology, University of Erlangen-Nuremberg, Germany
c
Department of Cariology, Endodontics and Pediatric Dentistry, School of Dental Medicine,
University of Geneva, Switzerland
d
Department of Oral Biology and Maxillofacial Pathology, Medical College of Georgia, Augusta, GA, USA
e
Department of Operative Dentistry, Endodontics and Dental Materials, Bauru School of Dentistry,
University of Sao Paulo, Sao Paulo, Brazil

Received 16 June 2003; received in revised form 8 October 2003; accepted 28 April 2004

KEYWORDS Summary Objectives: This study tested the hypothesis that single-bottle total-etch
Total-etch; adhesives are effective in reducing dentine permeability under in vivo conditions.
Two-step; Methods: Crown preparations on vital human teeth were performed under local
Vital dentine; analgesia as part of the treatment plan for prosthetic rehabilitation. Four single-
Dentinal fluid; bottle adhesives (Single Bond, 3M ESPE; Excite DSC, Ivoclar Vivadent; Prime and Bond
Permeability NT Dual-Cure, Dentsply DeTrey and One-Step, Bisco Inc.) were applied to the cut
dentine after acid-etching. Polyvinyl siloxane impressions were taken, using an ultra-
low viscosity impression material, of the smear layer-covered dentine before
applying the adhesives to deep vital dentine, and after adhesive placement.
Additional impressions were taken of the adhesive-sealed dentine following the
removal of the provisional prostheses after a 710 day period. Epoxy resin replicas of
the crown preparations were examined with scanning electron microscopy to
evaluate the extent of dentinal fluid transudation during pre-bonded, immediately
bonded and post-bonded periods. Results: Dentinal fluid transudation from localised
areas that were close to the dental pulp was universally observed from all epoxy resin
replicas, irrespective of the adhesive employed. The transudation of dentinal fluid
from the control smear layer-covered dentine of each crown preparation was
comparatively mild when compared to the extent that was observed after total-
etching and application of the single-bottle adhesive. Dentinal fluid droplets were
specifically located over the surface of the adhesive layer. Continuous transudation

* Corresponding author. Tel.: C852-2859-0251; fax: C852-2559-3803.

E-mail address: kfctay@netvigator.com (F.R. Tay).

0300-5712/$ - see front matter q 2004 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jdent.2004.04.006
612 F.R. Tay et al.

of dentinal fluid occurred even after the removal of the provisional prostheses, and
was considerably more profuse in subjects who opted for the fitting of the permanent
prostheses without the use of a local anaesthetic solution. Conclusion: Single-bottle
adhesives, because of their lack of a comparatively more hydrophobic bonding resin
layer, behave as permeable membranes after polymerisation. They permit the
continuous transudation of dentinal fluid and do not provide a hermetic seal in vital
deep dentine. Although the relatively slow rate of diffusion of dentinal fluid is
unlikely to result in post-operative cold sensitivity, it may interfere with the optimal
polymerisation of dual-cured or auto-cured composites or resin cements in both
direct and indirect restorations.
q 2004 Elsevier Ltd. All rights reserved.

Introduction adhesives, simplified two-step total-etch adhesives

An important goal in conservative dentistry is to
restore the peripheral seal of dentine that originally
exists prior to the removal of enamel.1 As the smear
layer and smear plugs account for 86% of the total
resistance to fluid movement in deep dentine2, an
impervious seal is not easily achieved when bonding
is performed with total-etch adhesives after the
removal of the smear layer.3,4 Dentinal tubules that
are rendered patent by acid-etching and rinsing
permit transudation of dentinal fluid from deep
dentine that are close to vital pulps.5,6 When
hydrophobic unfilled resins and composite restor-
ations were placed on vital acid-etched dentine,
expression of dentinal fluid droplets during the
polymerization of the resin composite resulted in
the manifestation of pits and blisters along the
intaglio surface of the restorations, being negative
impressions of the transudated dentinal fluid.7
Dentine bonding has been progressing rapidly
since the era when hydrophobic resins were used on
acid-etched dentine. Hydrophilic adhesive mono-
mers have been introduced during the past several
decades to ensure that contemporary dentine
adhesives are compatible with the intrinsic wetness
of dentine. 8,9 Both total-etch and self-etch
adhesives are available that enable clinicians to
bond effectively to dental substrates with or with-
out the removal of the smear layer.10 Simplified
versions of both total-etch and self-etch adhesives
have also been introduced into the market in
response to the clinicians desire for optimising
speed and efficiency in clinical practice.11
Conventional thought is that a perfect seal of the
resindentine interface can be established once the
dentinal tubules and spaces within the deminer-
alised collagen matrices are completely infiltrated
by adhesive resins. Such a notion is based on the
assumption that polymerised resins used for bond-
ing are nonporous and impermeable to fluid move-
ment. Unlike conventional three-step total-etch
or single-bottle adhesives, as they are generally
referred to, are directly coupled to resin compo-
sites without an additional coat of more hydro-
phobic bonding resin.10 This is similar to the
application of single-step self-etch adhesives in
two aspects. On one hand, the elimination of an
additional coating of bonding resin reduces the
overall thickness of the adhesive layer. On the other
hand, ionic (e.g. carboxyl and phosphate) and
hydrophilic (hydroxyl) groups that are originally
present in the adhesive monomers are retained
within the micro-domains of the adhesive layer.12,13
They may act as hydrophilic solids that continues
to draw water from the underlying vital dentine
after polymerisation.14 Because of their relatively
high permeability, single-step self-etch adhesives
were reported to behave as permeable membranes
after polymerisation,15,16 allowing the diffusion of
water from the hybridised dentine to the adhesive
surfaces. The phenomenon of increased adhesive
permeability has also been recently reported for a
single-bottle total-etch adhesive 17 , and was
thought to contribute partially, apart from adverse
acid-base reactions, for the incompatibility that
was observed between acidic simplified-step
adhesives and auto-cured resin composites that
utilized basic tertiary amines as catalytic
components.18
The assumption that adhesive-sealed dentine is
impermeable to water movement has resulted in
the effective use of single-bottle total-etch
adhesives in reducing cervical hypersensitivity via
resin-obliteration of exposed dentinal tubules.1922
Likewise, sealing of tooth preparations for indirect
restorations with dentine adhesives has been
advocated in fixed prosthodontics that involves
the preparation of vital teeth2326, since the use of
provisional cements may permit more microleakage
of bacteria and their products than the final
restorations.27,28 In view of the increased adhesive
permeability associated with simplified-step
Permeability of single-bottle adhesives
adhesives, it is not known whether a hermetic seal
can be achieved with the use of single-bottle total-
etch adhesives for the sealing of preparations for
indirect restorations in vivo. Of particular concern
is whether these adhesives can be effectively
employed for eliminating dentinal fluid movement
in freshly exposed, vital deep dentine that are close
to pulp horns, where the contribution of a positive
pulpal pressure is expected to be high.2931 Thus,
the objective of this study was to test the
hypothesis that single-bottle total-etch adhesives
are effective in reducing dentine permeability
under in vivo conditions.
Materials and methods
Sixteen vital posterior teeth (upper and lower
premolars and molars from 11 subjects) that
required crown preparations for fixed prosthodon-
tics were selected. The age of the subjects ranged
from 21 to 39 years. The distribution of the teeth by
arch and location is represented in the Table 1.
Informed consent of the subjects were obtained
under an in vivo protocols reviewed and approved
by the ethical committee from the University of
Geneva.
Experimental design
Four single-bottle total-etch dentine adhesives
were examined. They included two ethanol-based
adhesives (Single Bond, also known as Scotchbond
1, 3M ESPE, St. Paul, MN, USA, and Excite DSC,
Ivoclar Vivadent, Schaan, Liechtenstein), and two
acetone-based adhesives (Prime&Bond NT Dual-
Cure, Dentsply DeTrey, Konstanz, Germany, and
One-Step, Bisco Inc., Schaumburg, IL, USA). All the
adhesives were applied according to the manufac-
turers instructions. For Single Bond and One-Step,
two coats of adhesive were consecutively applied,
as suggested by the manufacturer. All adhesives
were checked to ensure complete wetting of the
etched dentine before light-activation. In addition,
a second layer of adhesive was applied after the
placement and light-curing of the first adhesive
layer. The rationale for the use of an additional
adhesive layer was that the oxygen inhibition layer
Table 1 Distribution of the crown preparations by
arch and location.
Premolars Molars
Maxillary 3 4
Mandibular 2 7
613
of the adhesives had to be removed prior to
impression taking for indirect restorations, a
procedure that is not usually performed for direct
restorations.32 This ensured that there was an
adequate layer of polymerised adhesive on the
sealed crown preparations when taking impressions
of the bonded surface.
In vivo procedures
Four teeth were randomly assigned to each
adhesive group. Crown preparations were per-
formed under infiltration or block analgesia that
were delivered using a local anaesthetic solution
containing a vasoconstrictor (2% mepivacaine
hydrochloride with 1:20,000 levonordefrin; Dents-
ply Pharmaceutical, York, PA, USA). Examination of
dentinal fluid transudation was performed using a
non-invasive epoxy resin replica protocol with each
tooth serving as its own control. Immediately after
crown preparation, an impression of the smear
layer-covered dentine was first taken with a low
viscosity polyvinyl siloxane impression material
(Affinis Light Body; Coltene/Whaledent, Altstatten,
Switzerland) that has an intraoral setting time of
3.5 min. The impression material was injected
directly onto the crown preparation without the
use of an impression tray, and was allowed to
polymerise without the use of additional heavy
body impression material. The crown preparation
was briefly air-dried for 1 s before the injection of
the impression material.
After taking the first research impression of the
smear layer-covered dentine, the crown prep-
arations were acid-etched with the bonding pro-
ducts respective phosphoric acid gels for 15 s,
thoroughly rinsed and maintained visibly moist.
Bonding was performed under an endodontic
microscope (OPMI pico, Carl Zeiss, Oberkochen,
Germany), with the two layers of adhesives light-
cured separately using a halogen light-curing unit
(VIP, Bisco Inc.) with an output of 600 mW/cm2.
The oxygen inhibition layer was gently removed
with a cotton pledget that was moistened with
water. The crown preparations were examined
under the endodontic microscope to ensure that
their surfaces were adequately covered with a
glassy layer of polymerised adhesive. As it has been
shown that taking impressions did not affect the
integrity of the bonded adhesive33, a second
research impression was taken of the adhesive-
coated crown preparation. Injection of the
impression material was performed under the
endodontic microscope, with the adhesive-coated
crown preparation briefly air-dried for 1 s to
614
remove any surface moisture or seepage of crevi-
cular fluid. After the research impressions were
taken, working impressions were then produced for
the construction of the fixed prostheses. Provisional
prostheses were luted using a non-eugenol provi-
sional cement (Temp-Bond NE, Sybron Kerr,
Orange, CA, USA).
The subjects were re-examined after 1014 days
for the fitting of the permanent restorations. Any
complaint on sensitivity to cold during the period of
temporization was noted. Following the removal of
the provisional prosthesis, each crown preparation
was gently hand-cleaned using a microbrush con-
taining a slurry of water and pumice to remove the
residues of the provisional cement. This procedure
was performed either with or without the use of
local analgesia, at the discretion of the individual
subject. A third research impression was taken of
the adhesive-coated dentine using the same
impression material prior to the fitting and cemen-
tation of the permanent prosthesis.
In vitro procedures
The research impressions were ultrasonically
cleaned in distilled water, degassed for 48 h, and
then poured up with a TEM grade epoxy resin (TAAB
812, TAAB Laboratories, Aldermaston, UK), follow-
ing the protocol reported by Itthagarun and Tay.6
The completely polymerised epoxy resin replicas
were then mounted on brass stubs, sputter-coated
with gold/palladium and examined with a scanning
electron microscope (Cambridge Stereoscan 360,
Cambridge, UK) operating at 20 kV. Both of occlusal
and buccal surfaces of each replica were examined.
Micrographs were recorded from the region of each
epoxy resin cast in which the most profuse
transudation of dentinal fluid was observed.
Results
None of the subjects reported any complaint of
severe post-operative cold sensitivity during the
period of provisional crown and bridge insertion.
The epoxy resin replicas of all the impressions taken
during pre-bonded, immediately bonded and post-
bonded periods provided an historical record of the
amount of dentinal fluid that transudated across
dentine during the setting time of the material.
Representative examples from crown preparations
bonded with each adhesive are shown in Fig. 1
(Single Bond), Fig. 2 (Prime&Bond NT Dual-Cure),
Fig. 3 (One-Step) and Fig. 4 (Excite DSC). When the
resin replicas from the same tooth were examined
F.R. Tay et al.
in sequence, transudation of dentinal fluid was
found to be non-uniform and localised to specific
regions, reflecting the variation in permeability
from different regions of a crown preparation.34
These regions corresponded with areas that were in
close proximity with the dental pulp.
For the same period of time that corresponded
with the setting time of the impression material,
the extent of dentinal fluid transudation in the
smear layer-covered dentine was comparatively
modest, and was limited to segregated, non-
coalesced droplets (Figs. 1A, 2A and 3A). Irrespec-
tive of the single-bottle adhesive employed, much
more transudation of dentinal fluid was observed
after total-etching and adhesive bonding (Figs. 1B,
2B and 3B). As the adhesives were applied to the
crown preparations without the additional coupling
of resin composites, there were no shrinkage
stresses that could result in the disruption of the
adhesives from the bonded dentine. A higher
magnification of the adhesive surface of
Single Bond revealed the absence of dentinal
tubules, and the presence of very fine droplets of
dentinal fluid that emerged directly from the
adhesive layer (Fig. 1C).
It was apparent from the sequential resin
replicas that removal of the provisional crowns
resulted in a continuous transudation of dentinal
fluid from the adhesive surfaces. The retention of
the adhesives over the crown preparations could be
confirmed by occasional disruptions of the adhesive
layer, with partial exposure of the underlying
dentine (Fig. 1D). For each individual crown
preparation, there was always more profuse fluid
transudation after the removal of the provisional
crown when compared with the control smear
layer-covered dentine. However, it was difficult to
determine whether the extent of transudation was
more or less profuse in the immediately bonded or
post-bonded dentine for the subjects who
requested for the teeth to be anaesthetised
during the fitting of the permanent restorations
(Fig. 2B vs. C). Conversely, in those subjects who
requested for crown-fitting to be performed with-
out local analgesia, extensive transudation could be
seen, as illustrated by an example from a tooth
bonded with One-Step (Fig. 3C). The entire area
observed in the micrograph was covered by dentinal
fluid droplets, obscuring the underlying adhesive
layer. The transudation was much greater than the
original adhesive-bonded dentine in which
impressions were taken under local analgesia
(Fig. 3B), which in turn, was more abundant than
the control smear layer-covered dentine (Fig. 3A).
The effect of the application of local
analgesia during the fitting and cementation of
Permeability of single-bottle adhesives 615

Figure 1 SEM micrographs of epoxy resin replicas of vital deep dentine in a crown preparation that was sealed with
single bond (3M ESPE) prior to impression taking. Local analgesia was employed during crown preparation, adhesive
application, and the subsequent removal of the provisional crown. The unbonded smear-layer-covered dentine from
each tooth served as the control. A. The surface of the unbonded smear layer-covered dentine (S), showing the presence
of sparse, dentinal fluid droplets (pointer) that transudated from the underlying dentinal tubules. B. The surface of the
adhesive-coated dentine (A) immediately after the removal of the oxygen inhibition layer. The adhesive coating did not
completely seal the dentine. Transudation of dentinal fluid through the adhesive occurred in areas adjacent to the pulp
horns. C. A high magnification view of the previous micrograph, showing the presence of very fine droplets of dentinal
fluid (open arrowheads) among the larger, partially coalesced droplets. D. Resin replica of an impression that was taken
from the same tooth after removal of the provisional crown that was luted with a non-eugenol type of provisional
cement. The crown preparation was gently hand-cleaned with a bonding brush and a slurry of pumice and water. The
adhesive layer was partially damaged during the cleaning procedure or impression taking, exposing the underlying
dentine (arrow). Transudation of dentinal fluid was still evident from deep dentine that was adjacent to the pulp horns.

the permanent prosthesis is vividly illustrated in
Fig. 4. The set of micrographs were taken from the
same buccal incline plane from the occlusal surface
of an upper left premolar that was bonded with two
coats of Excite DSC after crown preparation under
local analgesia. Fig. 4A represents the overall
picture of the adhesive-sealed inclined surface
that remained relatively clear of dentinal fluid
transudation, except for a localised region that was
adjacent to the pulp horn. In this particular region,
dentinal fluid transudation was fairly rapid, as could
be discerned by the partial coalescence of the
individual fluid droplets into larger droplets
(Fig. 4B). Fitting of the permanent prosthesis was
performed in the absence of local analgesia upon
the subjects request. There was only mild, toler-
able sensitivity on rinsing with water following the
removal of the provisional crown. However, when
the resin replica was examined, the entire buccal
inclined surface was laden with dentinal fluid
droplets (Fig. 4C). These droplets were smaller in
size and did not exhibit a tendency to coalesce into
616
Figure 2 SEM micrographs of epoxy resin replicas of
vital deep dentine in a crown preparation that was sealed
with Prime And Bond Nt Dual-Cure (Dentsply DeTrey)
prior to impression taking. Local analgesia was employed
during crown preparation, adhesive application, and
the subsequent removal of the provisional crown.
A. Unbonded smear layer-covered dentine (S) with sparse
dentinal fluid transudation. B. Adhesive-coated dentine
(A) immediately after bonding and removal of the oxygen
inhibition layer. More profuse dentinal fluid transudation
F.R. Tay et al.
larger droplets, indicating that the rate of transu-
dation was probably slower than that occurring
immediately after the crown preparation (Fig. 4D).
Discussion
We retained the use of the term single-bottle
adhesives in this study, as they are more commonly
known to clinicians than the use of two-step, self-
priming, total-etch adhesives. However, it is
pertinent to mention that many of these systems
(with the exception of One-Step) include an
additional bottle of activator solution containing
aryl sulphinate salts that are mixed with the single-
bottle adhesives to enable them to bond to dual-
cured or auto-cured resin composites or resin
cements. A generic aryl sulphinate salt-containing
solution is also available (BondLink, Dent-Mat,
Santa Maria, CA, USA) that is applied to the surface
of the cured single-bottle adhesives to achieve a
similar purpose.14 Thus, in the context of bonding
of indirect restorations, the term single-bottle
adhesive should be used with reservation.
The results of this in vivo study suggested that
single-bottle adhesives, irrespective of whether
they are ethanol-based or acetone-based, behave
as permeable membranes after polymerisation. The
complementary in vitro results that investigated
the permeability of these adhesives using fluid
conductance measurements4,35 and transmission
electron microscopy examination of the nanoleak-
age along the adhesivecomposite interfaces will be
reported in Part II of this series. Further exper-
iments should also be performed to determine the
electrical impedance of these hydrophilic adhesive
layers, when they are employed according to the
manufacturers instructions, or in combination with
more hydrophobic adhesive coatings.26,36 The
phenomenon of increased adhesive permeability is
similar to what was previously reported for single-
step self-etch adhesives16, and appears to be a
characteristic of simplified adhesives. This is
probably caused by the absence of a more hydro-
phobic bonding resin layer that is employed in
conventional total-etch and self-etch adhesives. It
is alarming to see that profuse transudation of
dentinal fluid occurred even when an additional
layer of the same type of single-bottle adhesive was
could be observed through the permeable adhesive layer.
C. Adhesive-coated dentine (A) following removal of the
provisional crown. A similarly profuse transudation of
dentinal fluid could be seen in areas that were close to
the pulp horns.
Permeability of single-bottle adhesives
Figure 3 SEM micrographs of epoxy resin replicas of
vital deep dentine in a crown preparation that was sealed
with One-Step (Bisco) prior to impression taking. Local
analgesia was employed during crown preparation and
adhesive application only. Removal of the provisional
crown was conducted without the use of local analgesia,
at the patients request. A Sparse transudation of
dentinal fluid from the unbonded smear layer-covered
dentine (S). B. More profuse dentinal fluid transudation
could be seen from the adhesive-coated surface (A)
immediately upon the removal of the oxygen inhibition
layer. C. Following the removal of the provisional crown,
617
applied and light-cured separately. In a recent
report in which the electrical resistance across
total-etch and self-etch adhesive layers was
measured before and after bonding, the electrical
resistance increased 315 fold after bonding com-
pared with the pre-coated smear layer-covered
dentine.26 The electrical resistance was further
increased by 5185 times after the application of a
second adhesive coating.26 In the same study, the
authors also pointed out that the increase in
electrical resistance was negligible when these
conventional adhesives were applied to dentine
without the use of the low viscosity bonding resin.
These results provided the rationale for the use of
the resin coating technique37,38when indirect
restorations were luted with Panavia F (Kuraray
Medical Inc., Tokyo, Japan), a resin cement that
employs a simplified self-etching primer (ED
primer) for bonding to hydrated dentine. In this
technique, the dentine is sealed with a two-step
self-etch adhesive and a light-cured, low viscosity
microfilled resin prior to impression taking. Indirect
restorations were subsequently luted to this resin-
coated tooth surface using Panavia F.
It should be pointed out that the observation of
profuse transudation of dentinal fluid across the
adhesive layer was not accompanied by severe
complaints of sensitivity to cold during the period
of temporisation. As water movement through the
polymerised adhesive layer involves slow diffusion
rather than rapid fluid transport through the
dentinal tubules39, it is unlikely that the A-delta
nerve endings within the pulp chamber will be
triggered to elicit sharp pain. This probably explains
why these adhesives are effective in reducing
cervical hypersensitivity. However, the results
indicated that all the single-bottle adhesives
examined did not provide a hermetic seal, and
were even less effective than the original smear
layer in protecting freshly cut, vital deep dentine. If
water and small ions can move across the
adhesives, one wonders what the molecular weight
cut-off will be to prevent permeation of noxious
substances.
Another potentially deleterious issue that is
associated with the transudation of dentinal fluid
across the polymerised adhesives is that these fluid
droplets may contribute to the incompatibility
between simplified adhesives and dual/auto-cured
composites in direct restorations, and the use
of resin cements for luting indirect restorations.
severe dentinal fluid transudation could be identified
from areas that were close to the pulp horn, almost
completely obscuring the underlying adhesive layer.
618 F.R. Tay et al.

Figure 4 SEM micrographs of epoxy resin replicas of vital deep dentine in a crown preparation that was sealed with
Excite DSC (Vivadent) prior to impression taking. Local analgesia was employed during crown preparation and adhesive
application only (A and B). Removal of the provisional crown was conducted without the use of local analgesia, at the
patients request (C and D). A. An overall view of the buccal incline of the adhesive-coated crown preparation (A)
showing minimal fluid transudation. B. A specific region along the buccal incline in which there was fairly profuse
dentinal fluid transudation, with coalescence of the adjacent droplets (arrows). The surrounding adhesive-coated
dentine (A) was devoid of fluid transudation. C. When the provisional crown was removed without the use of a local
anaesthetic, the entire buccal incline was laden with dentinal fluid droplets. D. These droplets were smaller in
dimensions and did not appear to coalesce.

As it takes time for water diffusion to occur across
the adhesives, transudation of dentinal fluid is
unlikely to affect the bonding of light-cured
composites. However, the 3.5 min intraoral setting
time of the polyvinyl siloxane impression material
approximates the slow setting time of dual/auto-
cured composites. Thus, it is possible that transu-
dated dentinal fluid will be trapped by the
dual/auto-cured composites when they are placed
over the adhesives in vital dentine. This may result
in the production of pits and blisters along the
intaglio surface of the restorations, similar to those
reported by Nordenvall.7 The blisters may act as
stress raisers and form initial flaws that precipitate
subsequent catastrophic failure along the adhesive
composite interfaces in minimally retentive cav-
ities. It has been shown that the incompatibility of
single-step self-etch with dual/auto-cured compo-
sites is contributed only partially by adverse acid
base reactions between the acidic resin monomers
and the basic tertiary amines employed as catalytic
components of these composites.16,40 As these
adhesives are also permeable to water and ion
movement, communication between the dental
pulp and oral environment still existed even in the
presence of hybridised smear plugs or resin tags.41
Using an in vitro protocol that consisted of the use
of light-cured composites with delayed light
Permeability of single-bottle adhesives
activation15, or auto-cured composites14 on these
simplified self-etch adhesives, water was found to
diffuse from the underlying hydrated dentine,
through the polymerized adhesive layer, and
deposit as water droplets along the adhesive
composite interface. The presence of these water
droplets may also interfere with bonding of indirect
restorations by inducing emulsion polymerisation
of the coupling hydrophobic resin cements16,42
and was thought to be a contributing factor
in the incompatibility between dual/auto-cured
composites/resin cements and simplified self-etch
adhesives, under the condition that then adverse
acidbase reaction between the acidic monomers
and basic tertiary amines was offset via the
inclusion of ternary catalytic systems.43 The
transudation of dentinal fluid through simplified
self-etch adhesives has also been demonstrated in
vivo, using a similar technique as that employed in
the present study (Chersoni et al., unpublished
results).
Likewise, it was previously assumed that the
incompatibility that existed between total-etch,
single-bottle adhesives and dual/auto-cured com-
posites was caused by acid-base incompatibility
alone.18 Although total-etch adhesives usually
contain lower concentrations of acidic (ionic)
resin monomers than self-etch adhesives, the
simplified versions of both total-etch and self-
etch adhesives are similar in that the hydrophilic
adhesive layers are not covered with a more
hydrophobic resin coating. It was recently
reported that adhesive permeability that contrib-
uted to adhesive/composite incompatibility was
also observed in OptiBond Solo Plus Dual-Cure
(Kerr Corp., Orange, CA, USA), a single-bottle
adhesive that utilises a sodium benzene sulphinate
activator to offset the adverse acid-base reac-
tions.17 The transudation of water through one-
step, as illustrated by the results of this study,
may provide an explanation for the 50% drop in
micro-tensile bond strength when this adhesive,
being the least acidic among the single-bottle
adhesives44, was used for bonding of auto-cured
composites.18 Both Sanares et al.18 and Dong
et al.44 reported that there was almost no bonding
when Prime&Bond NT bonded to hydrated dentine
was coupled with auto-cured composites. It would
be interesting to repeat the microtensile bond
testing of Prime&Bond NT Dual-Cure on hydrated
dentine using a dual-cured composite in either
the light-cured mode or auto-cured mode. By
eliminating the adverse acid-base reaction, any
observed drop in bond strength in the auto-cured
mode may be attributed to the increase in
619
permeability associated with the use of simplified
adhesives.
A speculation on how water movement occurs
through the polymerised adhesive layers is beyond
the scope of this in vivo study and will be discussed
in the in vitro part of this series. Clinically, it
appears that the use of solvated adhesives on vital
exposed dentine did not coagulate the plasma
proteins in the dentinal fluid enough to reduce
dentine permeability, as previously shown by
Nikaido et al.45 in an in vitro study. This is supported
by the continuous transudation of dentinal fluid
following the removal of the provisional prostheses
after a 710 day period. From the more profuse
transudation that occurred when provisional pros-
theses were removed without local analgesia,
clinicians may find it more appropriate to adminis-
ter a local anaesthetic to ensure optimised cemen-
tation of the permanent prostheses, even when
there is minimal complaint of sensitivity. In the
present study, the adhesives were used basically
according to the manufacturers instructions,
except for the application of the second coat of
the same adhesive. It is anticipated that the results
could be worse when only a single layer of adhesive
(notetwo consecutive coats for Single Bond) was
employed. Further in vivo studies should be
performed to evaluate if transudation of dentinal
fluid across single-bottle adhesives can be reduced
or eliminated by blocking dentinal tubules with
either glutaraldehyde-containing dentine desensi-
tisers46 that were reported to produce septa of
coagulated plasma proteins within the tubules47, or
the use of potassium oxalate solutions on acid-
etched dentine that resulted in the deposition of
calcium oxalate within the dentinal tubules.46,48 It
would also be of clinical interest to see if the
transudation of dentinal fluid can be reduced with
the adjunctive use of a more hydrophobic resin
coating over the single-bottle adhesives, such as
those employed in conventional three-step
systems.
Acknowledgements
We thank W.S. Lee of the Electron Microscopy
Unit, the University of Hong Kong for technical
assistance. This study was supported in part,
by grants from the Faculty of Dentistry, the
University of Hong Kong, and by grant DE014911
from the NIDCR, USA. The authors are grateful to
Zinnia Pang and Michelle Barnes for secretarial
support.
620
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