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Journal of Prosthodontic Research 54 (2010) 153158

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Original article

Effect of chlorhexidine application on long-term shear bond strength

of resin cements to dentin
Fereshteh Shafiei DMD, MSa, Mahtab Memarpour DMD, MSb,*
a

Operative Dentistry Department, Dental Faculty, Shiraz University of Medical Sciences, Shiraz, Iran
Pediatric Dentistry Department, Dental Faculty, Shiraz University of Medical Sciences, Shiraz, Iran

Received 20 October 2009; received in revised form 24 December 2009; accepted 28 January 2010
Available online 11 March 2010

Abstract
Purpose: The purpose of this study was to investigate the effect of chlorhexidine [CH] on dentin bond strength of three resin cements after 1 year
of water storage.
Methods: A flat middle dentin surface was prepared on 120 extracted premolars. The teeth were randomly divided into 6 groups of 20 specimens each
according to the resin cement used: Panavia F2.0, Variolink II, and RelyX Unicem, with or without CH application. After cementation of an indirect
composite rod [Z250], one subgroup [n = 10] was tested after 24 h in water at 37 8C and the other subgroup [n = 10] was tested after 1 year storage in
water plus thermocycling. A shear bond strength [SBS] test was performed. The data [in MPa] were analyzed with ANOVA and Tukey tests [P < 0.05].
Results: Three-way ANOVA [resin cement, CH and time] indicated that Variolink II had the highest strength [16.65  3.60] and RelyX Unicem
had the lowest strength [9.30  4.07]. Chlorhexidine application increased SBS [13.31  4.61] compared to samples without CH [12.16  5.04]
[P = 0.04]. Initial SBS [15.63  4.37] was significantly higher than after 1 year of storage [9.85  3.36] [P < 0.001]. Separate two-way ANOVA
for 24-h and 1-year data showed that cement had a significant effect but CH and its interaction had no significant effect at 24 h, whereas at 1 year the
two factors and their interaction differed significantly [P  0.001].
Conclusions: Chlorhexidine 2% can diminish the loss of bonding effectiveness over time associated to etch-and-rinse and self-etch cements,
although it appears not have any effect on self-adhesive cement.
# 2010 Japan Prosthodontic Society. Published by Elsevier Ireland. All rights reserved.
Keywords: Shear bond strength; Chlorhexidine; Resin cements

1. Introduction
Despite some advantages of indirect composite restorations
compared to direct composite [1], durable bonding of these
restorations to dentin is still a problem. Resin cements together
with adhesive systems are used to bond indirect restorations to
the tooth structure. These adhesives include both etch and rinse
or self-etch materials [2,3]. To reduce technique sensitivity and
simplify handling, self-adhesive cements were introduced in
2002, eliminating the need for pretreatment for both the tooth
and the restoration [4]. RelyX Unicem1 self-adhesive resin
cement is based on newly developed multifunctional phosphoric acid methacrylates that can react with the basic fillers in
the resin cement and the hydroxyapatite of the tooth [3]. During

* Corresponding author. Tel.: +98 711 6263193 4; fax: +98 711 6270325.
E-mail address: memarpour@sums.ac.ir (M. Memarpour).

cementation there are two interfaces, one between the resin

cement and the indirect restoration, and the other between the
adhesive system and dentin surface [3].
Integrity and stability of the bond at the complex interface
increase retention and fracture resistance of the restoration and
tooth structure [5,6], guaranteeing the long-term success of
adhesive indirect restorations. Roughening the fitting surface of
the composite by sandblasting, followed by silanization has
been recommended to increase bonding between the resin
cement and the indirect composite restoration [7].
Bonding failure at the adhesivedentin interface can lead to
microleakage, resulting in staining, recurrent caries and postoperative sensitivity [8]. Even if a complete seal is achieved
with a preparation, proliferation of entrapped bacteria
following incomplete sterilization of the preparation from
infected enamel and dentin can magnify the problems
associated with microleakage, causing pulpal inflammation
[9,10]. In etch-and-rinse adhesives, etching will increase the

1883-1958/$ see front matter # 2010 Japan Prosthodontic Society. Published by Elsevier Ireland. All rights reserved.
doi:10.1016/j.jpor.2010.01.005

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F. Shafiei, M. Memarpour / Journal of Prosthodontic Research 54 (2010) 153158

Table 1
Resin cement systems used and their application procedures.
Resin cement/
manufacturer

Adhesive system/
category

Component/bath#

Dentin pretreatment

Composite pretreatment

Luting agent mixing

Panavia F2.0

ED primer II
one-step
self-etch

ED primer A 00252
ED primer B 00129

Mix one drop of each

ED primer liquid A
and B for 5 s air dry
gently after 60 s.

Apply etchtant gel for 5 s,

rinse, air dry, mix one
drop of each Clearfil SE
primer and Porcelain Bond
Activator for 5 s, apply.

Mix universal and catalyst

paste for 20 s, light cure
for 20 s, after removal
excess cement, apply
oxyguard for 3 min.

Apply gel etchtant [37%

phosphoric acid] for 15 s,
rinse, air dry, apply excite
for 10 s, air dry and
light cure for 20 s.

Apply etchtant gel for 15 s,

rinse, air dry, apply
Monobond S for 60 s,
air dry.

Mix base and catalyst

past for 1020 s,
light cure for 20 s.

No pretreatment

No pretreatment

Mix the capsule for 15 s,

light cure for 20 s

Kuraray Inc.,
Tokyo, Japan
Variolink II

Universal paste 00269

Catalyst paste 00053
Excite DSC
two-step etch
and rinse

Ivoclar Vivadent Schaan,

Liechtenstein
RelyX Unicem 3M,
ESPE, USA

Excite DSC H34763

Base paste Catalyst

paste H34047
No adhesive

permeability of the tubules and possibility of bacterial invasion

[11]. With self-etch adhesives bacteria may remain in the smear
layer if etching is omitted [12].
Disinfecting of cavity surface with an antibacterial agent
such as chlorhexidine (CH) is beneficial in reducing the risk of
pulpal inflammation resulting form bacterial activity [13,14].
Apart from its antibacterial property, CH also has an inhibitory
effect on the matrix metalloproteinase (MMP) activity in
dentin. This effect can be useful in preventing collagen
degradation and disintegration of the bonding interface over
time [15,16]. Two important mechanisms are involved in the
loss of bond strength: hydrolytic degradation of hydrophilic
resin in the hybrid layer, and deterioration of the dentin
collagen fibrils [17,18]. Pretreating the cavity with CH during
luting of an indirect restoration may improve long-term
integrity of the dentin/cement interface.
Little information has been reported about the preservative
effect of CH on the dentin bond strength of resin cements.
Therefore, we decided to test the null hypotheses that 1) there is
no difference in long-term strength among three resin cements,
and 2) pretreatment of dentin with CH 2% associated to Panavia
F2.0 (self-etch adhesive), RelyX Unicem (self-adhesive) and
Variolink II (etch-and-rinse) cements does not affect their shear
bond strength after storage for 1 year.
2. Materials and methods
One hundred twenty sound human premolars extracted
because of orthodontic treatment were stored in a 1%
chloramine T solution for 2 weeks, then in distilled water at
4 8C before use. The roots were cut from the crowns 1-2 mm
below the cement-enamel junction using a diamond saw (Leitz
1600, Wetzlar, Germany). The teeth were then mounted in coldcured acrylic resin. The occlusal enamel was removed using a
diamond saw under a water spray to expose the midcoronal
dentin. The dentin surface was examined for lack of enamel or

pulp tissue under a stereomicroscope (Zeiss, Jena, Germany)

and polished with 600-grit carbide paper under water cooling to
provide a standardized smear layer. After ultrasonic cleaning,
washing and drying, adhesive tape with a 4-mm diameter hole
in it was used to define the bonding area.
The prepared teeth were then randomly divided into three
main groups according to the resin cement used: Panavia F2.0,
Variolink II, or RelyX Unicem [Table 1]. Each resin cement
was assigned to two control and CH application groups of 20
specimens each.
An indirect composite rod 2 mm in diameter and 3 mm in
height was incrementally built up with two layers of a
microhybrid resin composite (Filtek Z250, 3 M ESPE, St Paul,
MN, USA) in a split teflon mold. Each increment was lightcured at 600 mW/cm2 for 40 s using a light curing unit (VIP
Junior, Bisco, Schaumburg, IL, USA). Polymerization was
completed in an oven at 120 8C for 7 min. The surfaces for
bonding were sandblasted with 50-mm alumina particles
(Dento-Prep, Daugaard, Denmark), ultrasonically cleaned
and dried.
In control groups 1, 3 and 5, Panavia F2.0, Variolink II and
RelyX Unicem were used, respectively, as the resin cement for
luting indirect composites, according to the manufacturers
instructions [Table 1]. In experimental groups 2, 4 and 6, CH
2% (Consepsis Ultradent, South Jordan, Utah, USA) was
applied on the dentin surface for 60 s before ED Primer II in
Panavia F2.0, after acid etching in Variolink II and before selfadhesive resin cement in RelyX Unicem. In groups 2 and 6 the
dentin surface was air-dried for 10 s and in group 4, the dentin
surface was gently dried for 5 s.
Surfaces for indirect composite samples were prepared
according to the manufacturers instructions for each cement,
and cementation was done while applying a load of 500 g to
obtain the standard thickness of resin cement. Additionally,
light curing was performed for superior and lateral surfaces of
the bonded composite for 60 s at 600 mW/cm2 using a light

F. Shafiei, M. Memarpour / Journal of Prosthodontic Research 54 (2010) 153158

155

Table 2
Shear bond strength [Mean  SD], to dentin of three resin cements after 24 h
and 1 year.
Resin cement

Panavia F2.0 [self-etch]

Panavia F2.0 + chlorhexidine
Variolink II [etch-and-rinse]
Variolink II + chlorhexidine
RelyX Unicem [self-adhesive]
RelyX Unicem + chlorhexidine

Mean  SD (MPa)
24 h

One year

15.30  1.94
15.00  2.16
19.40  2.22
18.40  3.06
13.00  2.40
12.70  1.94

7.20  1.61
11.60  1.71
12.40  2.01
16.40  2.45
5.70  1.49
5.80  1.98

curing unit (VIP Junior). Half of the specimens (n = 10) in each

group were stored in tap water at 37 8C for 24 h and the other
half (n = 10) were stored in tap water (with stable pH 7.2  0.2)
at 37 8C for 1 year and additionally thermally cycled 1000
times between 5 8C and 55 8C with 20 s dwell time prior to
bond strength testing. Shear bond strength was measured using
a universal testing machine (Instron model 4302, Darmstadt,
Germany). A knife-edge sharing 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
effects of resin cement, CH and time. Then two separate twoway ANOVAs were performed after two storage periods (24 h
and 1 year) with two main factors: resin cement and the use of
CH or not. Multiple paired comparisons were done using Tukey
HSD post hoc tests. All tests were done at a 0.05 level
significance. After testing, the fracture modes were evaluated
under a stereomicroscope (Ziess) at 10, and classified
according to the predominant mode of fracture as adhesive
fracture at the resincement dentin interface, cohesive fracture
in the resin cement, cohesive fracture in dentin, or mixed
adhesive and cohesive fracture in the resin cement.
3. Results
The mean shear bond strengths and standard deviations in
the 12 experimental groups are presented in Table 2 and Fig. 1.
Three-way ANOVA revealed that bond strength was significantly influenced by the resin cement type (P < 0.001), CH
(P < 0.05), and time (P < 0.001). The interaction of these three
factors was also statistically significant (P = 0.029). The
highest overall bond strength (MPa) was observed with
Variolink II (16.65  3.60), followed by Panavia F2.0
(12.27  3.76), and RelyX Unicem had the lowest strength
(9.30  4.07). The use of CH led to a mean bond strength of
13.31  4.61, which was higher than without CH (mean
12.16  5.04, P = 0.04). The initial mean bond strength at 24 h
(15.63  4.37) was significantly higher than after 1 year
(9.85  3.36, P < 0.001).
Data analysis with two-way ANOVA for the 24-h results
with two main factors (type of cement and use or not of CH)
showed that type of cement had a significant effect, but CH and

Fig. 1. Box plot of dentin shear bond strength of different resin cements in the
12 experimental groups after 24 h and 1 year.

the interactions of these two factors did not have a significant

effect (P > 0.05). The highest bond strength was obtained with
Variolink II (18.90  2.65) followed by Panavia F2.0
(15.15  2.00) and RelyX Unicem (12.85  2.13). Tukeys
test indicated that there was a significant difference between
Panavia F2.0 and Variolink II (P < 0.001), between Panavia
F2.0 and RelyX Unicem (P < 0.05), and between Variolink II
and RelyX Unicem (P < 0.001).
Data analysis with two-way ANOVA for the 1-year results
with two main factors found that these two factors and their
interaction differed significantly (P < 0.001 and P = 0.001,
respectively). The highest bond strength was obtained with
Variolink II (14.40  2.99), followed by Panavia F2.0
(9.40  2.77) and RelyX Unicem (5.75  1.71). All paired
comparisons with Tukeys tests were significantly different
(P < 0.001). Mean bond strength with CH (11.27  4.84) was
significantly higher than without CH (8.43  3.36), although
CH had no effect when used with RelyX Unicem.
Fracture analyses indicated that most specimens showed
adhesive fractures. Only two specimens of Panavia F2.0 (with
CH) after 24 h showed a mixed fracture and two specimens of
Variolink II (without CH) after 24 h showed a cohesive fracture
in the dentin.
4. Discussion
Although the stress developed at adhesive interfaces in
indirect restorations is complex and there is no standard in vitro
method for reproduction [19,20], in vitro bond strength tests are
important in evaluating the strength of indirect restorations
[19]. Because many variables such as testing method, crosshead
speed, type of tooth, pulp pressure, dentin depth, bonding area
and conditions in the laboratory affect the results of bond

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F. Shafiei, M. Memarpour / Journal of Prosthodontic Research 54 (2010) 153158

strength tests, these tests are not reproducible [21]. Therefore,

direct comparisons of our results with previous studies [3,19
22] should be considered with due caution.
In the current study, we observed significant differences in
bond strength to dentin among the three resin cements after
24 h. This finding was also reported in earlier studies with
different resin cements [2227]. The chemical composition
of the resin cement and associated adhesive system is known
to affect dentin bond strength [23,25,2730]. In addition, it
was reported that shear bond strength was strongly
influenced by material properties such as elastic modulus
[31], and shear tests were the most efficient for determining
the cohesive strength of materials [32]. In contrast to our
results, Hikita and others reported equal microtensile bond
strength of etch-and-rinse, self-etch and self-adhesive resin
cements to dentin [3].
According to the manufacturers claim, RelyX Unicem does
not require dentin pretreatment. Although the pH of mixed
cement is initially very low (<2) [33], the smear layer and
underlying dentin probably rapidly buffer the acidity, thereby
limiting the etching ability of acidic monomers [34]. No
demineralization of the dentin surface was observed, and
infiltration of the resin into the collagen network was
insufficient. This transmission electron microscopy observation
might explain the lower bond strength of RelyX Unicem [33
35].
The major shortcoming of current adhesive systems is their
limited bonding durability [17].
This loss of strength in the resindentin bond is detrimental
to the longevity of indirect restorations luted using resin
cements. In the current study, the bond strengths of all three
resin cements decreased significantly after 1 year. Nevertheless,
the relative differences among cements after 1 year were the
same as after 24 h: Variolink II had the highest and RelyX
Unicem had the lowest bond strength. Thus, because we
detected differences in long-term strength between the
cements, the first part of the null hypotheses was rejected.
A decrease in bond strength after 1 year was observed by
Kitasako and others. According to these authors, the type of
resin cement and demineralizing agent used influenced the
durability of bonding to dentin [24]. Higher shear bond strength
of Variolink II/Excite DSC compared to self-etching and selfadhesive cements was reported after storage and thermocycling
[26,27].
In vitro studies based on water storage of the bonded
specimens found a 2355% reduction in bond strength [36].
Dissolution and loss of resin was responsible for the loss of
bond strength [17,18,37,38] and this effect was adhesivespecific [37]. Chemical degradation of the nonresin infiltrated
collagen fibrils also occurs [17,18,3638]. Resin degradation is
related to water sorption within the hybrid layer. The presence
of high concentration of hydrophilic acidic monomers in
simplified two-step etch-and-rinse and one-step self-etch
adhesives results in more permeability to water movement
[3940]. This adhesive permeability and water sorption may
compromise the long-term integrity of bonding interface
[36,41]. ED Primer II contains a high concentration of HEMA

[3050%] and two other hydrophilic monomers [MDP,5NMSA] in its composition. Water would react with HEMA to
form a hydrogel in the hybrid layer [42]. The presence of
HEMA can compromise the mechanical properties of the
polymers [43].
Water sorption caused a remarkable reduction in the elastic
modulus of the resins. This plasticizing of the resin may
contribute to the decrease in bond strength independently of
resin hydrolysis [40]. Earlier studies reported degradation of the
resindentin bond with ED Primer II after 1 year of storage [44]
and high permeability of the adhesive layer with Excite DSC
[45].
In the current study, RelyX Unicem was used without any
adhesive system. This cement contains a high concentration of
hydrophilic acidic monomers. This hydrophilicity can lead to
water uptake which can in turn result in swelling and
plasticizing of the resin cement [46]. The extent and rate of
water uptake depend on the formulation and density of the
polymer network and the potential for hydrogen bonding and
polar interactions [47,48]. During the storage period, the
storage water was changed daily to prevent bacterial growth as
was also done in the study by Kitasako at al. [24]. Daily changes
of the water might weaken the resindentin interface and might
be a way to accelerate the testing of long-term bond strength
[24].
In attempt to prevent hydrolytic degradation of collagen
matrices in aged dentinresin bonds, application of CH as an
MMP inhibitor during bonding procedures was suggested
[15,16]. Mild acids such as those found in simplified etch-andrinse and self-etch adhesives may activate MMPs [41,49,50].
These MMPs can reach the exposed collagen fibers at the base
of the hybrid layer in etch-and-rinse adhesive following
incomplete resin penetration within demineralized dentin
[36,38]. Incomplete resin impregnation was also observed
for self-etch adhesives, with the result that naked collagen in the
hybrid layer was affected by activated MMPs [51]. With
Panavia F 2.0 a self-etching primer (ED Primer II) is used
without any bonding resin; the relatively high-viscosity cement
acts as a bonding resin. Therefore, the presence of unprotected
collagen fibers is possible.
Because of these considerations, in the current study the
application of CH could diminish but not completely prevent
the loss of bond strength of etch-and-rinse cement (Variolink II)
and self-etch cement [Panavia F2.0] after 1 year. The decreased
bond strength in groups with CH was related to resin
hydrolysis.
The beneficial effect of CH on the bonding integrity of etchand-rinse adhesives such as Single Bond was reported
previously [5254]. In a study by Campos and others [55],
the preservative effect of CH 2% on bond strength of etch-andrinse and self-etch adhesives was reported during a 6-month
aging period. In the current study, CH had no effect on bonding
durability of RelyX Unicem. This cement was used on the
smear layer-covered dentin directly without any adhesive, and
its interaction with the dentin surface was very superficial.
Therefore, exposure of collagen and MMP activation in the
dentin may be not possible. Thus, the second part of the null

F. Shafiei, M. Memarpour / Journal of Prosthodontic Research 54 (2010) 153158

hypotheses was rejected for Variolink II and Panavia F2.0 but

confirmed for RelyX Unicem.
In the current study, CH did not affect the bond strengths of
three resin cements after 24 h. This finding was also observed in
direct adhesive restorations [10,54,56,57], although an adverse
effect of CH on bond strength was reported [58]. The lack of
adverse effects of CH was in agreement with other bond
strength studies of indirect restorations that used etch-and-rinse
cements [5961]. However, in a study by Hiraishi et al. [61], the
use of CH before Panavia F2.0 resulted in decreased bond
strength and increased nanoleakage. Their explanation was that
the adverse effect of CH may be attributed to the application of
CH to smear layer-covered dentin. Bonding CH to the loose,
superficial apatites within the smear layer could interfere with
the functions of the ED Primer monomers. In addition, 2% CH
solution is composed of 2% CH digluconate and 98% water.
After application of this solution residual moisture might
diminish the properties of functional monomers in ED Primer.
This latter effect was confirmed by de Castro and Andrade [56].
However, the dentin surface in the current study was air-dried
after the application of CH.
The present study was performed in a static environment on
the flat dentin surface. Clinically, numerous other factors affect
bond strength such as thermal, mechanical, chemical and
fatigue stress during function. Thus, further in vitro studies that
simulate the polymerization stress of resin cements in real
cavity preparation are needed. Even so, long-term clinical data
still need to evaluate the durability of bonding effectiveness of
resin cements used in indirect restorations.
The results of this in vitro study indicate that several
measures to simplify the application procedure of resin cements
resulted in decreased initial and long-term bonding effectiveness. Application of 2% CH could help preserve the bond
strength of etch-and-rinse and self-etch resin cements to dentin
after aging, but would probably not have any effect on self-etch
cements.
Acknowledgments
The authors thank Dr M. Vossoghi of the Center for
Development of Clinical Research of Namazee Hospital for the
statistical analysis, and K. Shashok (AuthorAID in the Eastern
Mediterranean) for help with the English in the manuscript.
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