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Journal of Prosthodontic Research 56 (2012) 187–193

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Original article
Effect of oxalate desensitizer on the bonding durability of
adhesive resin cements to dentin
Fereshteh Shafiei DMD, MScDa, Mahtab Memarpour DMD, MScDb,*,
Maryam Doozandeh DMD, MScDa
a
Operative Dentistry Department, Dental Faculty, Shiraz University of Medical Sciences, Shiraz, Iran
b
Pediatric Dentistry Department, Dental Faculty, Shiraz University of Medical Sciences, Shiraz, Iran
Received 26 April 2011; received in revised form 13 October 2011; accepted 21 November 2011
Available online 20 January 2012

Abstract
Purpose: This study investigated whether the tubular occluding effect of oxalate desensitizer (OX) during adhesive cementation improved
bonding of a self-etch and two etch-and-rinse resin cements to dentin after 6 months.
Methods: A flat dentin surface was prepared on 120 extracted premolars, which were randomly divided into six groups of 20 teeth each according
to the adhesive resin cement system used: ED primer II/Panavia F2.0, Excite DSC (Ex DSC)/Variolink II, and One-Step Plus (OS Plus)/Duolink,
with or without OX (BisBlock) application. After cementation of an indirect composite rod, two subgroups (n = 10) were tested after 24 h and 6
months of water storage plus thermocycling, and shear bond strengths were recorded in MPa.
Results: Statistical tests showed that although oxalate had a borderline significant negative effect on initial bonding of ED primer II/Panavia F2.0,
it significantly improved bonding durability ( p < 0.05). OX severely compromised the initial bond strength of Ex DSC/Variolink II ( p < 0.001)
but had no effect on the reduction in bonding after aging. OX was compatible with OS Plus/Duolink and did not affect the loss of bonding strength
after 6 months ( p > 0.05).
Conclusion: Combining an oxalate desensitizer with three types of resin cements had different effects on bond strength to dentin after aging,
depending on the interaction of oxalate with the adhesive system associated to the resin cement.
# 2011 Japan Prosthodontic Society. Published by Elsevier Ireland. All rights reserved.

Keywords: Desensitizer; Adhesive resin cements; Oxalate; Bond strength

1. Introduction after the luting of adhesive indirect restorations [4]. Gross

During recent years, patients’ increasing demands for esthetic
restorations and the development of many tooth-colored materials
have resulted in the wide use of indirect esthetic restorations.
These restorations are bonded to the tooth structure by adhesive
resin cements. The cements are resin cements together with
adhesive systems that used to bond indirect restorations to the
teeth structure [1,2]. Effective and durable bonding of resin
cements to restoration materials and the tooth structure are
necessary to guarantee a successful restoration. This bonding
reinforces both substrates, increases retention and decreases
microleakage, resulting in reduced postoperative sensitivity [2,3].
The most important postrestorative complication, which
poses a frequent problem in clinic practice, is hypersensitivity
* Corresponding author. Tel.: +98 711 6263193–4; fax: +98 711 6270325.
E-mail address: memarpour@sums.ac.ir (M. Memarpour).
reduction of the vital tooth structure during preparation for
indirect restoration exposes a large number of tubules. Etch-and-
rinse and self-etch adhesive systems, used to bond the resin
cement to the tooth structure [5], lead to sealing of the exposed
tubules. Simplified versions of these adhesives have been
marketed to provide simpler and faster adhesion procedures [6].
However, the outward flow of dentinal fluid from the tubules can
interfere with resin monomer infiltration, especially with etch-
and-rinse adhesives that remove the smear layer [7]. In addition,
simplified versions of the adhesives act as permeable membranes
by incorporating the solvated hydrophilic monomer, and lack a
separate hydrophobic layer [8,9]. Air drying the adhesive and the
use of solvated ionic comonomer mixtures of the adhesive induce
outward evaporative and osmotic fluid transudation, respectively,
before polymerization of the adhesive [10,11]. This transudation
through the hybrid and adhesive layers may entrap water blisters
along the adhesive-resin interface. During mastication, the

1883-1958/$ – see front matter # 2011 Japan Prosthodontic Society. Published by Elsevier Ireland. All rights reserved.
doi:10.1016/j.jpor.2011.11.003
188 F. Shafiei et al. / Journal of Prosthodontic Research 56 (2012) 187–193
resultant rapid fluid flow can cause post-operative sensitivity
[9,10,12]. Furthermore, after polymerization of the adhesive and
during slow setting of dual-cure resin cements, water can diffuse
from the underlying hydrated dentin across the simplified
adhesives via an osmotic gradient [8,13,14]. This water may
interfere with resin cement polymerization by inducing emulsion
polymerization of the hydrophobic luting resin cement [8,9,14].
This phenomenon is one of two main factors responsible for
the incompatibility between auto/dual-cured resin cements and
simplified adhesives [13,15]. As a result of water permeation,
bonded indirect restorations may become partially decoupled,
and bond strength will probably be reduced [8,9]. Moreover, the
lack of a hermetic seal at the adhesive interface can lead to
hypersensitivity subsequent to microleakage. Sustained seating
pressure may suppress water flow through a simplified self-etch
adhesive, thereby improving the final bond strength of self-etch
resin cements to the hydrated dentin [16].
Dentin hypersensitivity is reduced when the dentinal tubules
are intrinsically blocked by the precipitation of water-insoluble
materials [12,17]. Some components in dentin desensitizers
may induce chemical interactions with the dentin, impairing
subsequent interactions between the dentin and resin cement.
This interference may decrease the bond strength of resin
cements to desensitizer-treated dentin [17]. Some studies found
that various dentin desensitizers compromised the bond
strength of different luting cements to dentin [17–19].
Therefore, the best way to relieve post-operative sensitivity
is subsurface tubular occlusion with the application of
occluding agents that do not interfere with subsequent resin
infiltration or result in the formation of hybridized resin tags.
Tubular occlusion together with the formation of a hybrid layer
and resin tags ensure the creation of a double seal [20,21].
Oxalate desensitizer (OX, BisBlockTM, Bisco, Schaumburg,
USA) has been marketed as an acidic resin-free oxalate
potassium solution or gel. When OX is applied to the smear
layer-covered dentin, it replaces the smear layer with a layer of
crystals [12,19]. When OX is applied on acid-etched dentin,
calcium oxalate crystals occlude the dentin tubules 5–10 mm
below the surface, and the dentin surface is available for bonding
with adhesives. Therefore, OX does not compromise the bond
strength of relatively neutral etch-and-rinse adhesives [22–24].
The potential advantage of tubular occlusion during bonding with
adhesive resin cements is that it limits interference with resin
infiltration by tubular fluid flow and facilitates solvent and water
evaporation [21,23]. Thus, OX enhances the formation of a
homogenous hybrid layer throughout the whole depth of the
demineralized wet dentin. These benefits may increase the
durability of cements bonded to hydrated dentin. In this
connection, the occluding effect of OX was reported to reduce
the incompatibility between a simplified etch-and-rinse adhesive,
One-Step Plus (OS Plus, Bisco, Schaumburg, USA) and auto-
curing or light-curing resin cements in the delayed polymeriza-
tion mode [25]. The reduced permeability to water was
responsible for the beneficial effects of OX pretreatment [23,25].
No studies to date have investigated the effect of the
combination of OX with adhesive cements on their long-term
bonding effectiveness to dentin. We therefore designed this
study to evaluate the effect of OX application before
cementation on the initial and middle-term bond strength of
three adhesive resin cements. The null hypothesis was that
combining OX with adhesive resin cements during cementation
would have no effect on their bond strength to dentin 24 h after
cementation in indirect restoration, or after water storage for 6
months plus thermocycling.
2. Materials and methods
One hundred and twenty noncarious human premolars
extracted for orthodontic treatment were used in this study. The
protocol of the experiment was approved by the local ethics
committee for human studies. The teeth were stored in a 1%
chloramine T solution at 37 8C for 2 weeks, and then stored in
distilled water at 4 8C before use. The roots were removed from
the crowns 2 mm below the cemento-enamel junction (CEJ)
with a diamond saw (Leitz 1600, Wetzlar, Germany) under
water cooling, then the crowns were horizontally mounted in
autocured acrylic resin.
The midcoronal dentin surfaces were exposed by removing
the occlusal enamel with a diamond saw under a water spray.
The dentin surfaces were examined under a stereomicroscope
(Zeiss, Jena, Germany) to ensure that no enamel or pulp tissue
remained. The flat dentin surfaces were polished with 600 grit
silicon carbide abrasive paper to provide a standardized smear
layer. After ultrasonic cleaning, rinsing and drying, adhesive
tape with a 4-mm diameter hole in it was applied to the prepared
surfaces to limit the bonding area. The prepared teeth were
randomly divided into three main groups according to the resin
cement used: ED primer II/Panavia F2.0 (Kuraray Medical,
Tokyo, Japan), Excite DSC (Ex DSC)/Variolink II (Ivoclar
Vivadent Schaan, Liechtenstein), or One-Step Plus (OS Plus)/
Duolink. Each resin cement was assigned to two control and
OX application groups of 20 teeth each.
An indirect composite rod 2 mm in diameter and 3 mm in
height was incrementally built up with two layers of an indirect
composite (Gradia, GC, Tokyo, Japan) in a split teflon mold. Each
increment was light-cured for 40 s at 600 mW/cm2 with a light-
curing unit (VIP Junior, Bisco, Schaumburg, USA). Polymeriza-
tion was completed in a GC LaboLight LV-III (Leuven, Belgium)
for 3 min. The composite rod surface for bonding was
sandblasted with 50-mm aluminum particles (Dento-Prep,
Daugaard, Denmark), cleaned ultrasonically and dried.
In control groups 1, 3 and 5, Panavia F 2.0, Variolink II and
Duolink resin cements were used, respectively, as the resin
cement for luting indirect composites, according to the
manufacturer’s instructions. In experimental groups 2, 4 and
6, OX (BisBlock, Bisco) was added to bonding procedures. In
group 2, OX was first applied and dwelled onto the dentin
surfaces for 30 s, the surfaces were rinsed for 60 s and dried,
then ED primer II was applied followed by Panavia F2.0. In
group 4, after acid etching, OX was applied, then the surfaces
were rinsed for 60 s and dried, then Ex DSC/Variolink II was
applied. In group 6, after acid etching, OX was applied and the
surfaces were rinsed for 60 s and dried, then OS Plus was
applied, followed by Duolink resin cement. In group 2, after
 F. Shafiei et al. / Journal of Prosthodontic Research 56 (2012) 187–193 189

Table 1
Resin cement systems used and their application procedure.
Resin cement/batch#/ Chemical component Adhesive system/ Dentin pretreatment Composite pretreatment Luting agent mixing
manufacturer batch#/category
Panavia F2.0 MDP, hydrophobic aromatic ED primer II Mix one drop of each Etch for 5 s, rinse, air dry, Mix universal and
Paste A/00447A dimethacrylate, hydrophobic A/00286A ED primer liquid A and mix one drop of each catalyst paste for
Paste B/00080A aliphatic dimethacrylate, B/00160B B for 5 s, air dry gently Clearfil SE primer and 20 s, light cure for
Kuraray Medical, hydrophilic aliphatic one-step after 60 s Porcelain Bond Activator 20 s, after removing
Tokyo, Japan dimethacrylate, silica filler, self-etch for 5 s, apply excess cement, apply
colloidal silica, Oxyguard for 3 min
DL-camphorquinone
Variolink II/K10496 Bis-GMA, triethyleneglycol Excite DSC Etch for 15 s, rinse, gently Etch for 15 s, rinse, air dry, Mix base and catalyst
Ivoclar Vivadent dimethacrylate, M52582 air dry, apply the adhesive apply Monobond S for 60 s, paste for 10–20 s,
Schaan, urethane dimethacrylate, Two-step etch for 10 s, air dry and light air dry light cure for 20 s
Liechtenstein dibenzoyl peroxide and rinse cure for 20 s
Duolink Bis-GMA triethyleneglycol One-Step Etch for 15 s, rinse, gently Etch for 15 s, rinse, air dry, Mix base and catalyst
09000011311/Bisco, dimethacrylate, Plus/0800004236 air dry. Shake the bottle for apply Monobond S for 60 s, paste for 10–20 s,
Schaumburg, USA urethane dimethacrylate Two-step 3–5 s. Apply two consecutive air dry light cure for 20 s
glass filler etch and rinse coats, agitate 20 s, gently air
dry, light cure for 10 s
Phosphoric acid, 3 M, Phosphoric acid gel (35%) Apply for 15 s, rinse 15 s,
ESPE, USA air dry for 10 s
MDP: methacryloyloxydecyl dihydrogen phosphate. Bis-GMA: bisphenol A-glycidyl methacrylate.

Table 2
Composition and pH value of adhesive systems associated to resin cements.
Adhesive system Composition pH
ED primer II A: HEMA, 10-MDP, 5-NMSA, water and accelerator 3
B: 5-NMSA, accelerator, water and sodium benzene sulfinate
Excite DSC Liquid: HEMA, dimethacrylates, phosphonic acid acrylate, silicon dioxide, initiators, stabilizers and ethanol 2.35
Microbrush: coated with initiators
One-Step Plus BPDM, Bis-GMA, HEMA, p-dimethylaminobenzoic acid, glass fillers and acetone 4.61
HEMA: hydroxyethyl methacrylate. MDP: methacryloyloxydecyl dihydrogen phosphate. NMSA: N-methacryloyl-5-aminosalicylic acid. BPDM: biphenyl
dimethacrylate. Bis-GMA: bisphenol A-glycidyl methacrylate.

rinsing for 60 s, the dentin surfaces were air-dried for 10 s and
in groups 4 and 6, the dentin surfaces were gently dried for 5 s,
leaving the dentin moist.
Surfaces for indirect composite samples were prepared
according to the manufacturer’s instructions for each resin
cement (Table 1), and cementation was performed while
applying a load of 500 g to obtain the standard thickness of
resin cement. Additionally, light curing was done for the
superior and lateral surfaces of the bonded composite for 60 s at
600 mW/cm2 with a light-curing unit (VIP Junior).
After the restorative procedures, half of the specimens
(n = 10) in each group were stored in distilled water at 37 8C for
24 h and the other half (n = 10) were stored in distilled water
containing 0.4% sodium azide with a stable pH at 37 8C for 6
months and additionally thermocycled 1000 times (between
5 8C and 55 8C with 20-s dwell times) prior to bond strength
testing. Shear bond strength was measured with a universal
testing machine (Instron model 4302, Darmstadt, Germany). A
knife-edge shearing rod at a crosshead speed of 1 mm/min was
used to load the specimens until fracture. Shear bond strength in
MPa was calculated from the peak load at failure divided by the
specimen surface area.
All data were analyzed with three-way ANOVA for the
effect of resin cement, OX and storage time. Bonferroni
adjustment tests were used to examine differences among
the groups. For each cement, a two-way ANOVA was done
to evaluate the effect of OX, storage time and interaction
of these two factors on bond strength of the three resin
cements. All tests were done at a 0.05 level of significance
and all analysis were performed using SPSS version 11.5
software (Chicago, IL, USA). After testing, the fracture
modes were evaluated under a stereomicroscope (Zeiss) at
10 and classified according to the predominant mode of
fracture as adhesive fracture at the resin cement–dentin
interface, cohesive fracture in the resin cement, cohesive
fracture in the dentin, or mixed adhesive and cohesive
fracture in the resin cement. The pH of the adhesive systems
associated to the resin cements was measured with a pH
meter [26].
3. Results
The pH of the adhesive systems associated to the resin
cements is presented in Table 2. The mean bond strengths and
190 F. Shafiei et al. / Journal of Prosthodontic Research 56 (2012) 187–193
Table 3
Shear bond strength (mean  SD) to dentin of three resin cements in control groups and groups pretreated with oxalate after 24 h and 6 months and fracture mode.
Resin cement system
Mean  SD (MPa)
A C
ED primer II/Panavia F 2.0 (control) 13.27  1.91
ED primer II/Panavia F 2.0 + OX 11.80  1.88B
Ex DSC/Variolink II (control) 15.73  1.74a
Ex DSC/Variolink II + OX 5.21  1.77c
OS Plus/Duolink (control) 13.66  1.931
OS Plus/Duolink + OX 13.01  1.571
For each resin cement, subgroups with the different superscripts are statistically significant. A: adhesive fracture. Cr: cohesive fracture in the resin cement. Cd:
cohesive fracture in the dentin. M: mixed adhesive and cohesive fracture in the resin cement.
standard deviations in the 12 experimental groups are
summarized in Table 3.
Three-way ANOVA showed significant differences in bond
strength between the three resin cements ( p < 0.001), and also
detected significant differences depending on storage time
( p < 0.001) and on whether OX was used or not ( p < 0.001).
Statistically significant interactions were found between type of
resin cement and use of OX ( p < 0.001), type of resin cement
and storage time ( p < 0.05), and use of OX and storage time
( p < 0.001). However, the interactions among all three factors
were not statistically significant ( p = 0.178).
The bond strengths of the three cements were significantly
reduced after 6 months of storage ( p < 0.001). In teeth treated
with ED primer II/Panavia F2.0, OX had a significant negative
effect on bond strength after 24 h ( p = 0.048), but diminished
the loss of bonding strength after 6 months ( p = 0.002). The
percentage reduction in bond strength was 34% in the control
group and 9% in the OX-treated group.
The combination of Ex DSC/Variolink II with OX resulted in
significantly lower bond strength than the control group (Ex
DSC/Variolink II without OX) ( p < 0.001), but OX had no
significant effect on the loss of bond strength after storage
( p > 0.05). After aging, the reduction in bond strength in the
two groups; with OX and control; was 55% and 26%,
respectively. In teeth treated with OS Plus/Duolink, OX exerted
no significant influence on initial bond strength or loss of bond
strength over time ( p < 0.05), and led to similar reductions
(approximately 21%) in both groups.
The results of fracture analysis indicated that all fractures in
the Ex DSC/Variolink II group with OX at both time periods were
adhesive fractures. In the 10 remaining groups, approximately all
four modes of fracture were observed (Table 3).
4. Discussion
The results of the current study demonstrated different
effects of OX on the initial and middle-term bonding
performance of three resin cements, and appear to reject the
null hypothesis. The application of OX to acid-etched dentin
before cementation with Ex DSC/Variolink II resulted in a
significant reduction (77%) in the initial bond strength, whereas
the oxalate desensitizer had no effect on the bond strength of
OS Plus/Duolink. We attribute this finding to the different pH of
24 h 6 months
Fracture A/Cr/Cd/M Mean  SD (MPa) Fracture A/Cr/Cd/M
5/2/0/3 10.12  1.25 7/1/0/2
5/1/1/3/ 10.83  2.12BC 8/0/0/2
4/2/0/4 11.64  2.25b 7/0/0/3
9/0/0/1 2.35  0.85d 10/0/0/0
6/2/0/2 10.74  1.682 5/0/0/5
5/1/1/3 10.38  1.992 6/2/0/2
the two simplified etch-and-rinse adhesives associated to the
resin cements. The low pH of Ex DSC (pH = 2.35) may have
dissolved the calcium oxalate crystals formed in the dentinal
tubules, compromising the formation of hybridized resin tags
and the hybrid layer. Moreover, the ethanol content as a solvent
in this adhesive may increase the solubility of calcium oxalate
in an ethanol–water mixture [27]. This adverse effect on the
sealing ability of the composite restoration bonded with low-pH
Excite was reported in a previous study [26].
Ex DSC is a dual-cure version of Excite with similar
components, except that Ex DSC has an additional initiator
coated on the brush supplied in the package. Earlier work
found that the tubular blocking capacity of OX treatment on
acid-etched dentin deteriorated after the low-pH fluoride-
containing adhesives were applied [28], and that this reduced
their bond strength [29]. This incompatibility may be related to
the formation of spherical globules (CaF2 material) following
interaction of the free fluoride ions present in the adhesives
with calcium and phosphate ions on the dentin surface. The low
pH of the adhesive is critical for this interaction because the
dentin surface is completely depleted of calcium phosphate
after acid etching. The calcium ions may have become
available from the dissolution of calcium oxalate crystals by
the low-pH adhesives [28,29]. In agreement with these reports,
OX pretreatment associated with OS Plus/Duolink in the
current study did not alter the bond strength of the Duolink
cement to dentin. The OS Plus adhesive, which is less acidic
(pH = 4.61), contains fluoride (806 ppm) [26]. This finding
was consistent with the manufacturer’s instructions, which
recommend the application of BisBlock in combination with
One-Step or One-Step Plus. One recent study reported that OX,
when applied with OS Plus, had no negative effect on the
sealing ability of composite restorations [26]. Two dentin
permeability studies [22,28] and three bond strength studies
[22,23,29] found that One-Step (which contains no fluoride)
was compatible with two or three resin-free oxalates. Also, the
combination OX with One-Step was found to be clinically
effective in relieving dentin hypersensitivity [30]. In a recent
study, the compatibility One-Step Plus/Variolink II with OX
resulted in a beneficial occluding effect of OX. This effect
reduced the adverse effect of tubular fluid flow on dentin bond
strength when chemical curing or delayed light curing of the
resin cement were used [25].
 F. Shafiei et al. / Journal of Prosthodontic Research 56 (2012) 187–193
Our findings showed that OX pretreatment resulted in an
11% reduction ( p = 0.048) in the bond strength of ED primer II/
Panavia F2.0 to dentin compared to the control group. This
effect was not found by Huh et al. [19], who reported no
significant difference (17% reduction) in shear bond strength
between the control group (Panavia F2.0) and the experimental
group treated with Superseal OX solution. The application of
low-pH OX on smear layer-covered dentin followed by rinsing
resulted in removal of the smear layer and replacement with
calcium oxalate crystals [12,19]. Huh et al. [19] suggested that
this effect may have permitted ED primer II to react directly on
the dentin, and their scanning electron microscopic (SEM)
observations showed that some tubules were covered and others
were not. Open tubules on the dentinal surface showed that
oxalate particles had penetrated the tubules, allowing the
formation of resin tags [19]. In a SEM study by Kolker et al.
[31], approximately half of the tubules appeared to be closed. A
dense crystal precipitate was in intimate contact with the tubule
wall, and tubules were visible funneling towards the dentin
surface. Although the tubules were blocked by the formation of
insoluble crystals on the peritubular dentin, the dentin surfaces
and openings of some tubules remained available to some
extent for hybrid layer formation.
The methacryloxydecyl dihydrogen phosphate (MDP)
content of ED primer II may give rise to a chemical interaction
with calcium in the calcium oxalate crystals on the dentinal
surface and intratubular walls. The formation of a hardly
soluble calcium salt may contribute to the beneficial effect of
OX on the bonding durability of ED primer II/Panavia F2.0 to
dentin, as found in the current study. Intimate monomer–dentin
interaction would be expected to extend bonding durability.
Furthermore, the partial tubular occluding effect of OX may
limit water permeation from the tubules, preventing water from
interfering with resin polymerization.
In general, bonding durability relies on the formation of a
well-polymerized, compact, homogenous hybrid layer [32,33].
As previously mentioned that OX may have an adverse effect
on the formation of a hybrid layer and hybridized resin tags by
Ex DSC/Variolink II, and this may account for a tendency to
negative effect of OX on bonding durability. It seems that the
lower bond strength in the Ex DSC/Variolink II group with
oxalate in both time periods was associated with adhesive
fracture at the resin cement–dentin interface. However, in the
other groups with higher bond strength, all four modes of
fracture were observed.
In the OS Plus/Duolink group, OX had no effect on initial and
middle-term bond strength. We surmise that OX did not interfere
with the ability of this adhesive to form bonds and had no effect
on the long-term mechanisms of bonding degradation in the OS
Plus/Duolink system. High water sorption by hydrophilic
adhesive resins can cause hydrolysis of the resin from
interfibrillar spaces within the hybrid layer. Water sorption
can also significantly decrease the elastic modulus of the resin.
Both of these effects can weaken the resin–dentin bond [32,34].
Incomplete hybridization and water exposure are the main
contributing factors to the degradation of resin–dentin bonds
[35]. Moreover, the presence of the adjacent composite–enamel
191
bond has a protective effect against the degradation of resin–
dentin bonds [36,37].
In the current study, circumferential resin–dentin margins
were directly exposed to water during storage, so water could
have penetrated from the storage media via the permeable
marginal hybrid layer [38] to the resin–dentin interface. This
water permeation may be a major factor in the degradation of
the resin at the interface. Our experimental design exaggerated
the clinical situation in which dentinal margins of indirect
restorations are exposed directly to the oral fluid. Nevertheless,
in in vivo, when perfect enamel sealing prevents direct exposure
of the resin–dentin interface to water, water transudation from
the dentinal tubules through the permeable hybrid and adhesive
layers of simplified adhesives plays a larger role in the
degradation of resin and unprotected collagen. Although the
solubility of hydrophilic calcium oxalate is low, it can
solubilize from the dentin surface within 1 week [22]. With
simultaneous resin degradation, calcium oxalate crystals may
dissolve gradually during water storage or under pulpal
pressure. The solubility behavior of oxalate crystals may differ
depending on the source of water exposure from external
sources, dentinal fluid or both. In a study by Vachiramon et al.
[39], reduced bond durability of a combination of OX with
Single Bond was attributed to the solubility of calcium oxalate,
which eventually created nanoleakage pathways and weakened
the bond. However, this study did not evaluate initial bond
strengths, so it is not clear whether the reduced bonding after
aging resulted from an adverse effect of OX on initial bonding
performance. In the present study we found this effect in the
group treated with a combination of Ex DSC and OX.
In a recent study [40], OX application together with Single
Bond resulted in decreased initial and long-term bond strength,
but with Prime and Bond NT, OX had no effect on initial
bonding or loss of bond strength after water storage for one
year. Despite the lower pH of Prime and Bond NT than Single
Bond, the apparent compatibility OX with Prime and Bond NT
has been attributed to different solvent contents in the two
adhesives and the fast vitrification rate of Prime and Bond NT,
which leads to more complete curing than with Single Bond
after initial curing.
In partially contrast with our results and those of Almeida
et al. [40], De Andrade e Silva et al. [41] reported that despite
the relatively high pH values and lack of fluoride content in the
three adhesives used in their study, OX compromised the initial
bond strength of Single Bond, One-Step and Adper Scotchbond
Multi-Purpose. However, OX application reduced the loss of
bond strength over time. The authors of the latter study [41]
suggested that the remaining oxalic acid after rinsing could
impair adhesive polymerization. In addition, the application
acidic oxalate after acid dentin etching had additional etching
effects. This overetching may have significantly decreased
dentin bond strength. However, transmission electron micro-
scopic observations in a recent study [39] did not support this
hypothesis, and further research will be needed to compare the
demineralization depth after acid etching with and without OX
treatment. Moreover, the discrepancy between the extent of
demineralization and penetration of the adhesive monomer as a
192 F. Shafiei et al. / Journal of Prosthodontic Research 56 (2012) 187–193
result of overetching can compromise not only the initial
bonding but also bonding durability [35,42]. This latter effect is
due to hydrolysis of the unprotected and incompletely resin-
coated collagen fibrils [43].
One of the possible limitations of our study design is that the
experiments were done with extracted teeth without a perfusion
system to simulate pulpal pressure. However, water perme-
ability could have occurred when the teeth were retrieved from
the water storage medium and immediately bonded in their
normal hydrated condition. As a result, permeability through
the tubules was less than permeability under pulpal pressure.
This work cannot completely predict the clinical behavior of
OX with resin cements in in vivo situations. Unless there is
direct scientific evidence how OX reacts with adhesive resin
cements, the clinician should not use this method prior to
cementation of indirect restorations. It seems that the effect of
OX pretreatment on the bonding durability of resin cements to
dentin may depend on the initial effect of OX on the bonding
performance of the adhesive associated to the resin cement, and
on the composition of the adhesive in terms of pH, solvent type
and specific monomer content. Dissolution of the calcium
oxalate crystals and the resin component of the hybrid layer
upon exposure to water may influence dentin bond strength
after aging.
5. Conclusion
The application of an oxalate desensitizer had a negative
effect on initial bond strength of the Panavia F2.0 system but
had a beneficial effect on bonding durability. The use of oxalate
severely decreased bonding strength of the Variolink II system
with no effect on bonding durability. In the Duolink system,
oxalate showed no effect on initial or long-term bonding.
Acknowledgments
The authors thank the Vice-Chancellory of Shiraz University
of Medical Science for supporting this research (Grant # 89-
5427). Also the authors thank Dr. M. Vossoughi of the Center
for Development of Clinical Research of Namazee Hospital for
statistical analysis, and K. Shashok, AuthorAID in the Eastern
Mediterranean for help with the English in the manuscript.
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