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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


reduction of the vital tooth structure during preparation for
During recent years, patients’ increasing demands for esthetic indirect restoration exposes a large number of tubules. Etch-and-
restorations and the development of many tooth-colored materials rinse and self-etch adhesive systems, used to bond the resin
have resulted in the wide use of indirect esthetic restorations. cement to the tooth structure [5], lead to sealing of the exposed
These restorations are bonded to the tooth structure by adhesive tubules. Simplified versions of these adhesives have been
resin cements. The cements are resin cements together with marketed to provide simpler and faster adhesion procedures [6].
adhesive systems that used to bond indirect restorations to the However, the outward flow of dentinal fluid from the tubules can
teeth structure [1,2]. Effective and durable bonding of resin interfere with resin monomer infiltration, especially with etch-
cements to restoration materials and the tooth structure are and-rinse adhesives that remove the smear layer [7]. In addition,
necessary to guarantee a successful restoration. This bonding simplified versions of the adhesives act as permeable membranes
reinforces both substrates, increases retention and decreases by incorporating the solvated hydrophilic monomer, and lack a
microleakage, resulting in reduced postoperative sensitivity [2,3]. separate hydrophobic layer [8,9]. Air drying the adhesive and the
The most important postrestorative complication, which use of solvated ionic comonomer mixtures of the adhesive induce
poses a frequent problem in clinic practice, is hypersensitivity outward evaporative and osmotic fluid transudation, respectively,
before polymerization of the adhesive [10,11]. This transudation
* Corresponding author. Tel.: +98 711 6263193–4; fax: +98 711 6270325. through the hybrid and adhesive layers may entrap water blisters
E-mail address: memarpour@sums.ac.ir (M. Memarpour). 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 study to evaluate the effect of OX application before
[9,10,12]. Furthermore, after polymerization of the adhesive and cementation on the initial and middle-term bond strength of
during slow setting of dual-cure resin cements, water can diffuse three adhesive resin cements. The null hypothesis was that
from the underlying hydrated dentin across the simplified combining OX with adhesive resin cements during cementation
adhesives via an osmotic gradient [8,13,14]. This water may would have no effect on their bond strength to dentin 24 h after
interfere with resin cement polymerization by inducing emulsion cementation in indirect restoration, or after water storage for 6
polymerization of the hydrophobic luting resin cement [8,9,14]. months plus thermocycling.
This phenomenon is one of two main factors responsible for
the incompatibility between auto/dual-cured resin cements and 2. Materials and methods
simplified adhesives [13,15]. As a result of water permeation,
bonded indirect restorations may become partially decoupled, One hundred and twenty noncarious human premolars
and bond strength will probably be reduced [8,9]. Moreover, the extracted for orthodontic treatment were used in this study. The
lack of a hermetic seal at the adhesive interface can lead to protocol of the experiment was approved by the local ethics
hypersensitivity subsequent to microleakage. Sustained seating committee for human studies. The teeth were stored in a 1%
pressure may suppress water flow through a simplified self-etch chloramine T solution at 37 8C for 2 weeks, and then stored in
adhesive, thereby improving the final bond strength of self-etch distilled water at 4 8C before use. The roots were removed from
resin cements to the hydrated dentin [16]. the crowns 2 mm below the cemento-enamel junction (CEJ)
Dentin hypersensitivity is reduced when the dentinal tubules with a diamond saw (Leitz 1600, Wetzlar, Germany) under
are intrinsically blocked by the precipitation of water-insoluble water cooling, then the crowns were horizontally mounted in
materials [12,17]. Some components in dentin desensitizers autocured acrylic resin.
may induce chemical interactions with the dentin, impairing The midcoronal dentin surfaces were exposed by removing
subsequent interactions between the dentin and resin cement. the occlusal enamel with a diamond saw under a water spray.
This interference may decrease the bond strength of resin The dentin surfaces were examined under a stereomicroscope
cements to desensitizer-treated dentin [17]. Some studies found (Zeiss, Jena, Germany) to ensure that no enamel or pulp tissue
that various dentin desensitizers compromised the bond remained. The flat dentin surfaces were polished with 600 grit
strength of different luting cements to dentin [17–19]. silicon carbide abrasive paper to provide a standardized smear
Therefore, the best way to relieve post-operative sensitivity layer. After ultrasonic cleaning, rinsing and drying, adhesive
is subsurface tubular occlusion with the application of tape with a 4-mm diameter hole in it was applied to the prepared
occluding agents that do not interfere with subsequent resin surfaces to limit the bonding area. The prepared teeth were
infiltration or result in the formation of hybridized resin tags. randomly divided into three main groups according to the resin
Tubular occlusion together with the formation of a hybrid layer cement used: ED primer II/Panavia F2.0 (Kuraray Medical,
and resin tags ensure the creation of a double seal [20,21]. Tokyo, Japan), Excite DSC (Ex DSC)/Variolink II (Ivoclar
Oxalate desensitizer (OX, BisBlockTM, Bisco, Schaumburg, Vivadent Schaan, Liechtenstein), or One-Step Plus (OS Plus)/
USA) has been marketed as an acidic resin-free oxalate Duolink. Each resin cement was assigned to two control and
potassium solution or gel. When OX is applied to the smear OX application groups of 20 teeth each.
layer-covered dentin, it replaces the smear layer with a layer of An indirect composite rod 2 mm in diameter and 3 mm in
crystals [12,19]. When OX is applied on acid-etched dentin, height was incrementally built up with two layers of an indirect
calcium oxalate crystals occlude the dentin tubules 5–10 mm composite (Gradia, GC, Tokyo, Japan) in a split teflon mold. Each
below the surface, and the dentin surface is available for bonding increment was light-cured for 40 s at 600 mW/cm2 with a light-
with adhesives. Therefore, OX does not compromise the bond curing unit (VIP Junior, Bisco, Schaumburg, USA). Polymeriza-
strength of relatively neutral etch-and-rinse adhesives [22–24]. tion was completed in a GC LaboLight LV-III (Leuven, Belgium)
The potential advantage of tubular occlusion during bonding with for 3 min. The composite rod surface for bonding was
adhesive resin cements is that it limits interference with resin sandblasted with 50-mm aluminum particles (Dento-Prep,
infiltration by tubular fluid flow and facilitates solvent and water Daugaard, Denmark), cleaned ultrasonically and dried.
evaporation [21,23]. Thus, OX enhances the formation of a In control groups 1, 3 and 5, Panavia F 2.0, Variolink II and
homogenous hybrid layer throughout the whole depth of the Duolink resin cements were used, respectively, as the resin
demineralized wet dentin. These benefits may increase the cement for luting indirect composites, according to the
durability of cements bonded to hydrated dentin. In this manufacturer’s instructions. In experimental groups 2, 4 and
connection, the occluding effect of OX was reported to reduce 6, OX (BisBlock, Bisco) was added to bonding procedures. In
the incompatibility between a simplified etch-and-rinse adhesive, group 2, OX was first applied and dwelled onto the dentin
One-Step Plus (OS Plus, Bisco, Schaumburg, USA) and auto- surfaces for 30 s, the surfaces were rinsed for 60 s and dried,
curing or light-curing resin cements in the delayed polymeriza- then ED primer II was applied followed by Panavia F2.0. In
tion mode [25]. The reduced permeability to water was group 4, after acid etching, OX was applied, then the surfaces
responsible for the beneficial effects of OX pretreatment [23,25]. were rinsed for 60 s and dried, then Ex DSC/Variolink II was
No studies to date have investigated the effect of the applied. In group 6, after acid etching, OX was applied and the
combination of OX with adhesive cements on their long-term surfaces were rinsed for 60 s and dried, then OS Plus was
bonding effectiveness to dentin. We therefore designed this 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 All data were analyzed with three-way ANOVA for the
in groups 4 and 6, the dentin surfaces were gently dried for 5 s, effect of resin cement, OX and storage time. Bonferroni
leaving the dentin moist. adjustment tests were used to examine differences among
Surfaces for indirect composite samples were prepared the groups. For each cement, a two-way ANOVA was done
according to the manufacturer’s instructions for each resin to evaluate the effect of OX, storage time and interaction
cement (Table 1), and cementation was performed while of these two factors on bond strength of the three resin
applying a load of 500 g to obtain the standard thickness of cements. All tests were done at a 0.05 level of significance
resin cement. Additionally, light curing was done for the and all analysis were performed using SPSS version 11.5
superior and lateral surfaces of the bonded composite for 60 s at software (Chicago, IL, USA). After testing, the fracture
600 mW/cm2 with a light-curing unit (VIP Junior). modes were evaluated under a stereomicroscope (Zeiss) at
After the restorative procedures, half of the specimens 10 and classified according to the predominant mode of
(n = 10) in each group were stored in distilled water at 37 8C for fracture as adhesive fracture at the resin cement–dentin
24 h and the other half (n = 10) were stored in distilled water interface, cohesive fracture in the resin cement, cohesive
containing 0.4% sodium azide with a stable pH at 37 8C for 6 fracture in the dentin, or mixed adhesive and cohesive
months and additionally thermocycled 1000 times (between fracture in the resin cement. The pH of the adhesive systems
5 8C and 55 8C with 20-s dwell times) prior to bond strength associated to the resin cements was measured with a pH
testing. Shear bond strength was measured with a universal meter [26].
testing machine (Instron model 4302, Darmstadt, Germany). A
knife-edge shearing rod at a crosshead speed of 1 mm/min was 3. Results
used to load the specimens until fracture. Shear bond strength in
MPa was calculated from the peak load at failure divided by the The pH of the adhesive systems associated to the resin
specimen surface area. 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 24 h 6 months
Mean  SD (MPa) Fracture A/Cr/Cd/M Mean  SD (MPa) Fracture A/Cr/Cd/M
A C
ED primer II/Panavia F 2.0 (control) 13.27  1.91 5/2/0/3 10.12  1.25 7/1/0/2
ED primer II/Panavia F 2.0 + OX 11.80  1.88B 5/1/1/3/ 10.83  2.12BC 8/0/0/2
Ex DSC/Variolink II (control) 15.73  1.74a 4/2/0/4 11.64  2.25b 7/0/0/3
Ex DSC/Variolink II + OX 5.21  1.77c 9/0/0/1 2.35  0.85d 10/0/0/0
OS Plus/Duolink (control) 13.66  1.931 6/2/0/2 10.74  1.682 5/0/0/5
OS Plus/Duolink + OX 13.01  1.571 5/1/1/3 10.38  1.992 6/2/0/2
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 the two simplified etch-and-rinse adhesives associated to the
summarized in Table 3. resin cements. The low pH of Ex DSC (pH = 2.35) may have
Three-way ANOVA showed significant differences in bond dissolved the calcium oxalate crystals formed in the dentinal
strength between the three resin cements ( p < 0.001), and also tubules, compromising the formation of hybridized resin tags
detected significant differences depending on storage time and the hybrid layer. Moreover, the ethanol content as a solvent
( p < 0.001) and on whether OX was used or not ( p < 0.001). in this adhesive may increase the solubility of calcium oxalate
Statistically significant interactions were found between type of in an ethanol–water mixture [27]. This adverse effect on the
resin cement and use of OX ( p < 0.001), type of resin cement sealing ability of the composite restoration bonded with low-pH
and storage time ( p < 0.05), and use of OX and storage time Excite was reported in a previous study [26].
( p < 0.001). However, the interactions among all three factors Ex DSC is a dual-cure version of Excite with similar
were not statistically significant ( p = 0.178). components, except that Ex DSC has an additional initiator
The bond strengths of the three cements were significantly coated on the brush supplied in the package. Earlier work
reduced after 6 months of storage ( p < 0.001). In teeth treated found that the tubular blocking capacity of OX treatment on
with ED primer II/Panavia F2.0, OX had a significant negative acid-etched dentin deteriorated after the low-pH fluoride-
effect on bond strength after 24 h ( p = 0.048), but diminished containing adhesives were applied [28], and that this reduced
the loss of bonding strength after 6 months ( p = 0.002). The their bond strength [29]. This incompatibility may be related to
percentage reduction in bond strength was 34% in the control the formation of spherical globules (CaF2 material) following
group and 9% in the OX-treated group. interaction of the free fluoride ions present in the adhesives
The combination of Ex DSC/Variolink II with OX resulted in with calcium and phosphate ions on the dentin surface. The low
significantly lower bond strength than the control group (Ex pH of the adhesive is critical for this interaction because the
DSC/Variolink II without OX) ( p < 0.001), but OX had no dentin surface is completely depleted of calcium phosphate
significant effect on the loss of bond strength after storage after acid etching. The calcium ions may have become
( p > 0.05). After aging, the reduction in bond strength in the available from the dissolution of calcium oxalate crystals by
two groups; with OX and control; was 55% and 26%, the low-pH adhesives [28,29]. In agreement with these reports,
respectively. In teeth treated with OS Plus/Duolink, OX exerted OX pretreatment associated with OS Plus/Duolink in the
no significant influence on initial bond strength or loss of bond current study did not alter the bond strength of the Duolink
strength over time ( p < 0.05), and led to similar reductions cement to dentin. The OS Plus adhesive, which is less acidic
(approximately 21%) in both groups. (pH = 4.61), contains fluoride (806 ppm) [26]. This finding
The results of fracture analysis indicated that all fractures in was consistent with the manufacturer’s instructions, which
the Ex DSC/Variolink II group with OX at both time periods were recommend the application of BisBlock in combination with
adhesive fractures. In the 10 remaining groups, approximately all One-Step or One-Step Plus. One recent study reported that OX,
four modes of fracture were observed (Table 3). when applied with OS Plus, had no negative effect on the
sealing ability of composite restorations [26]. Two dentin
4. Discussion permeability studies [22,28] and three bond strength studies
[22,23,29] found that One-Step (which contains no fluoride)
The results of the current study demonstrated different was compatible with two or three resin-free oxalates. Also, the
effects of OX on the initial and middle-term bonding combination OX with One-Step was found to be clinically
performance of three resin cements, and appear to reject the effective in relieving dentin hypersensitivity [30]. In a recent
null hypothesis. The application of OX to acid-etched dentin study, the compatibility One-Step Plus/Variolink II with OX
before cementation with Ex DSC/Variolink II resulted in a resulted in a beneficial occluding effect of OX. This effect
significant reduction (77%) in the initial bond strength, whereas reduced the adverse effect of tubular fluid flow on dentin bond
the oxalate desensitizer had no effect on the bond strength of strength when chemical curing or delayed light curing of the
OS Plus/Duolink. We attribute this finding to the different pH of resin cement were used [25].
F. Shafiei et al. / Journal of Prosthodontic Research 56 (2012) 187–193 191

Our findings showed that OX pretreatment resulted in an bond has a protective effect against the degradation of resin–
11% reduction ( p = 0.048) in the bond strength of ED primer II/ dentin bonds [36,37].
Panavia F2.0 to dentin compared to the control group. This In the current study, circumferential resin–dentin margins
effect was not found by Huh et al. [19], who reported no were directly exposed to water during storage, so water could
significant difference (17% reduction) in shear bond strength have penetrated from the storage media via the permeable
between the control group (Panavia F2.0) and the experimental marginal hybrid layer [38] to the resin–dentin interface. This
group treated with Superseal OX solution. The application of water permeation may be a major factor in the degradation of
low-pH OX on smear layer-covered dentin followed by rinsing the resin at the interface. Our experimental design exaggerated
resulted in removal of the smear layer and replacement with the clinical situation in which dentinal margins of indirect
calcium oxalate crystals [12,19]. Huh et al. [19] suggested that restorations are exposed directly to the oral fluid. Nevertheless,
this effect may have permitted ED primer II to react directly on in in vivo, when perfect enamel sealing prevents direct exposure
the dentin, and their scanning electron microscopic (SEM) of the resin–dentin interface to water, water transudation from
observations showed that some tubules were covered and others the dentinal tubules through the permeable hybrid and adhesive
were not. Open tubules on the dentinal surface showed that layers of simplified adhesives plays a larger role in the
oxalate particles had penetrated the tubules, allowing the degradation of resin and unprotected collagen. Although the
formation of resin tags [19]. In a SEM study by Kolker et al. solubility of hydrophilic calcium oxalate is low, it can
[31], approximately half of the tubules appeared to be closed. A solubilize from the dentin surface within 1 week [22]. With
dense crystal precipitate was in intimate contact with the tubule simultaneous resin degradation, calcium oxalate crystals may
wall, and tubules were visible funneling towards the dentin dissolve gradually during water storage or under pulpal
surface. Although the tubules were blocked by the formation of pressure. The solubility behavior of oxalate crystals may differ
insoluble crystals on the peritubular dentin, the dentin surfaces depending on the source of water exposure from external
and openings of some tubules remained available to some sources, dentinal fluid or both. In a study by Vachiramon et al.
extent for hybrid layer formation. [39], reduced bond durability of a combination of OX with
The methacryloxydecyl dihydrogen phosphate (MDP) Single Bond was attributed to the solubility of calcium oxalate,
content of ED primer II may give rise to a chemical interaction which eventually created nanoleakage pathways and weakened
with calcium in the calcium oxalate crystals on the dentinal the bond. However, this study did not evaluate initial bond
surface and intratubular walls. The formation of a hardly strengths, so it is not clear whether the reduced bonding after
soluble calcium salt may contribute to the beneficial effect of aging resulted from an adverse effect of OX on initial bonding
OX on the bonding durability of ED primer II/Panavia F2.0 to performance. In the present study we found this effect in the
dentin, as found in the current study. Intimate monomer–dentin group treated with a combination of Ex DSC and OX.
interaction would be expected to extend bonding durability. In a recent study [40], OX application together with Single
Furthermore, the partial tubular occluding effect of OX may Bond resulted in decreased initial and long-term bond strength,
limit water permeation from the tubules, preventing water from but with Prime and Bond NT, OX had no effect on initial
interfering with resin polymerization. bonding or loss of bond strength after water storage for one
In general, bonding durability relies on the formation of a year. Despite the lower pH of Prime and Bond NT than Single
well-polymerized, compact, homogenous hybrid layer [32,33]. Bond, the apparent compatibility OX with Prime and Bond NT
As previously mentioned that OX may have an adverse effect has been attributed to different solvent contents in the two
on the formation of a hybrid layer and hybridized resin tags by adhesives and the fast vitrification rate of Prime and Bond NT,
Ex DSC/Variolink II, and this may account for a tendency to which leads to more complete curing than with Single Bond
negative effect of OX on bonding durability. It seems that the after initial curing.
lower bond strength in the Ex DSC/Variolink II group with In partially contrast with our results and those of Almeida
oxalate in both time periods was associated with adhesive et al. [40], De Andrade e Silva et al. [41] reported that despite
fracture at the resin cement–dentin interface. However, in the the relatively high pH values and lack of fluoride content in the
other groups with higher bond strength, all four modes of three adhesives used in their study, OX compromised the initial
fracture were observed. bond strength of Single Bond, One-Step and Adper Scotchbond
In the OS Plus/Duolink group, OX had no effect on initial and Multi-Purpose. However, OX application reduced the loss of
middle-term bond strength. We surmise that OX did not interfere bond strength over time. The authors of the latter study [41]
with the ability of this adhesive to form bonds and had no effect suggested that the remaining oxalic acid after rinsing could
on the long-term mechanisms of bonding degradation in the OS impair adhesive polymerization. In addition, the application
Plus/Duolink system. High water sorption by hydrophilic acidic oxalate after acid dentin etching had additional etching
adhesive resins can cause hydrolysis of the resin from effects. This overetching may have significantly decreased
interfibrillar spaces within the hybrid layer. Water sorption dentin bond strength. However, transmission electron micro-
can also significantly decrease the elastic modulus of the resin. scopic observations in a recent study [39] did not support this
Both of these effects can weaken the resin–dentin bond [32,34]. hypothesis, and further research will be needed to compare the
Incomplete hybridization and water exposure are the main demineralization depth after acid etching with and without OX
contributing factors to the degradation of resin–dentin bonds treatment. Moreover, the discrepancy between the extent of
[35]. Moreover, the presence of the adjacent composite–enamel demineralization and penetration of the adhesive monomer as a
192 F. Shafiei et al. / Journal of Prosthodontic Research 56 (2012) 187–193

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of Medical Science for supporting this research (Grant # 89- [23] Tay FR, Pashley DH, Mak YF, Carvalho RM, Lai SC, Suh BI. Integrating
5427). Also the authors thank Dr. M. Vossoughi of the Center oxalate desensitizers with total-etch two-step adhesive. J Dent Res
for Development of Clinical Research of Namazee Hospital for 2003;82:703–7.
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GM. Microtensile bond strengths of composite to dentin treated with
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