Bond Strength Durability of Different Adhesives to Dentin

After Aging in Two Different Solutions

Heba A. El-Deeba / Lamia E. Daifallab / Omar I. Badran0/ Enas H. Mobarakd

Purpose: To determine the influence of aging in artificial saliva compared to distilled water on the dentin microtensile bond strength (pTBS) of different adhesive systems.
Materials and Methods: Occlusal enamel and superficial dentin of 42 teeth were removed and roots were sec
tioned to expose the pulp chamber for connecting the tooth segments to an intrapulpal pressure assembly. Accord
ing to the tested adhesives, tooth segments were allocated to three groups (n = 14): an etch-and-rinse adhesive
(Adper Scotchbond Multi-Purpose, SBMP), a two-step self-etching adhesive (Clearfil SE Bond, CSE), and a singlestep self-etching adhesive (Clearfil S3 Bond, S3). Each adhesive system was applied to the dentin surface accord
ing to its manufacturers instructions, while intrapulpal pressure was simulated. Resin composite (3M ESPE) was
built up in two increments of 2 mm each. Each bonded specimen was sectioned to obtain eight sticks
(0.8 0.01 mm2*). Sticks of each group were divided equally (n = 56) according to the storage solution, either dis
tilled water or artificial saliva. For each storage solution, half of the sticks of each subgroup (n = 28) was stored
for 24 h at 37C and the other half was thermocycled for 10,000 cycles between 5C and 55C. Sticks were then
subjected to pTBS testing. Data were statistically analyzed using multifactor ANOVA with repeated measures and
Bonferronis post-hoc test (p < 0.05). Students t-test was used for pairwise comparison. Failure modes were de
termined for all tested sticks using scanning electron microscopy.
Results: The decrease in bond strength of the three adhesives was significantly higher in distilled water than in ar
tificial saliva. The predominant failure modes were adhesive and mixed.
Conclusion: The decrease in bond strength was more pronounced for specimens stored in distilled water than in

artificial saliva.
Keywords: distilled water, artificial saliva, adhesives, dentin bonding, bond strength, storage, microtensile bond

strength.
J Adhes Dent 2016; 18: 303-309.
doi: 10.3290/].jad.a36153

uring the last decades, adhesive dentistry has fo

cused on enhancing bonding to dentin. Dental manu
facturers achieved te c h n ic a l59 and chem ical ad
vances15'61 to develop new dental adhesives with

3 Associate Professor, Restorative Dentistry Department, Faculty of Oral and

Dental Medicine, Cairo University, Egypt. Idea, performed the experiment,
wrote the manuscript.
b Associate Professor, Restorative Dentistry Department, Faculty of Oral and
Dental Medicine, Cairo University, Egypt. Contributed substantially to conduct
ing the study, co-wrote manuscript.
c PhD Student, Restorative Dentistry Department, Faculty of Oral and Dental Medi
cine, Cairo University, Egypt. Performed the experiment, co-wrote manuscript.
d Professor, Restorative Dentistry Department, Faculty o f Oral and Dental Medi
cine, Cairo University, Egypt. Hypothesis, experimental design, constructed
setups, contributed substantially to discussion, proofread the manuscript.
Correspondence: Enas H. Mobarak, Cairo University, Faculty o f Dentistry,
709 El-Malak El Saleh, Cairo, 1 1 5 5 0 Egypt. Tel: + 0020-2-2206-6203;
e-mail: enasmobarak@hotmail.com

Vol 18, No 4, 2016

Submitted for publication: 22.01.15; accepted for publication: 26 .041 6

increased resin-dentin bond strength. Currently, several

adhesive systems are available, from the multi-step ver
sions of etch-and-rinse and self-etching adhesives to the
more simplified single-step self-etching adhesives. Flowever, the loss of resin-dentin bond strength overtime still
affects the adhesive restorations and markedly reduces
their durability in vitro.8
To understand the causes behind bond degradation of
the adhesives being continually launched into the market,
both in vitro and in vivo experiments have been carried
out. The oral cavity is considered the ultimate testing en
vironment to reveal the behavior of the adhesives, al
though there diverse factors work simultaneously, making
it difficult to assess each factors contribution to bond
degradation separately. Flowever, in vitro models simulat
ing certain in vivo conditions can provide less complex en
vironments to assess the fundamental mechanisms of
bond degradation.55

303

El Deeb et al

Fig 1 Specimen preparation for

intrapupal pressure simulation: ob
taining the coronal section (a);
cleaning of the pulp chamber (b);
Teflon plate fixation (c); butterfly
needle insertion and embedding of
the specimen (d); bonded speci
mens in the specially constructed
incubator while connected to intrapulpal pressure assembly (e).

For instance, many studies have used distilled water as

a storage solution for short- or even long-term periods to
assess bond durability.11'1417223536'39-40'5460 Others
preferred to mimic the clinical situation and used artificial
saliva as an immersion solution.6'8232443 Furthermore, in
laboratory settings, thermocycling is used as a model at
tempting to test bond degradation. It allows bonded speci
mens to be subjected to extreme temperatures. Previous
articles1016 suggested that 1 0,000 thermocycles corre
spond to approximately one year of in vivo functioning.
Nevertheless, whether the interaction between artificial sa
liva as a storage solution, used alone or in combination
with the thermocycling process, and adhesive restorations
would differ from that of distilled water storage solution has
yet to be validated.
Therefore, the current study was performed to examine
the influence of artificial saliva, with or without thermocy
cling, compared to distilled water, on the bond strength dura
bility of adhesives with different bonding strategies to dentin.
The null hypotheses were: 1) there is no difference between
dentin microtensile bond strengths when specimens are
stored for 24 h in distilled water vs artificial saliva; 2) there
is no difference between dentin microtensile bond strengths
with or without thermocycling; 3) there is no difference be
tween dentin microtensile bond strengths when thermocycled
either in distilled water or in artificial saliva.

MATERIALS AND METHODS

Specimen Preparation
A total of 42 sound human third molars were selected for
the study. Selected teeth were stored in phosphate buffer
solution containing 0.02% sodium azide at 4C until being
used.
Each tooth was attached upside down with its occlusal
surface placed on the center of a circle drawn on a glass

304

slab to facilitate centrally embedding it in a chemically cur

ing polyester resin (Polyester # 2 1 2 1 , Eternal Chemical;
Hsein, Taiwan), leaving the crown and 1 to 2 mm of hard
tooth structure gingival to the cementoenamel junction ex
posed using the same protocol described previously by
Mobarak et al.33 This was done to facilitate trimming the
tooth perpendicular to its longitudinal axis using a dia
mond disk (Isomet, Buehler; Lake Bluff, IL, USA) under a
stream of water to remove occlusal enamel and superficial
dentin to obtain a flat dentin surface (midcoronal portion).
A second cut was made parallel to the occlusal surface,
2 mm gingival to the cementoenamel junction, thereby ex
posing the pulp chamber (Fig la ). Remnants of pulp tissue
in the pulp cham ber were removed using an excavator
(Carl M artin; Solingen, Germany) w ithout touching the
walls of the pulp chamber (Fig lb ) .48 Dentin surfaces were
then wet polished using 600-grit silicon carbide paper (MicroCut, 8 inch, Buehler) for 10 s to produce a standard
ized smear layer and surface roughness.32 Then, the spec
im ens were connected to th e intra pu lpa l pressure
assembly during bonding (Fig 1 c-e) following the same
procedures described by Mobarak.30

Restorative Procedures
Prepared specimens were divided into three groups (n = 14)
according to the tested adhesives: an etch-and-rinse adhe
sive, Adper Scotchbond Multi-Purpose (SBMP, 3M ESPE;
St Paul, MN, USA); a two-step self-etching adhesive, Clearfil
SE Bond (CSE, Kuraray Noritake; Tokyo, Japan); and a sin
gle-step self-etching adhesive, Clearfil S3 Bond (S3, Kuraray
Noritake). Each adhesive system was applied according to
the manufacturers instructions (Table 1) while intrapulpal
pressure was simulated. Resin composite (Filtek Z250, 3M
ESPE) shade A3 was applied in two increments of 2 mm
each, each of which was polymerized for 20 s using Bluephase C5 (Ivoclar Vivadent; Schaan, Liechtenstein) with an
intensity of > 500 m W /cm 2. Light intensity was checked

The Journal of Adhesive Dentistry

El Deeb et al
Table 1

Material specifications, manufacturers, compositions, and application procedures

M a te r ia l (m a n u fa c tu r e r )

C o m p o s itio n

A p p lic a tio n p r o c e d u r e s
E tchant: Apply fo r 1 5 s, rinse w ith w a te r spray fo r 1 5 s,
th e n dry w ith g e n tle a ir flo w fo r 5 s.

Adper S cotchb ond M ulti-Purpose,

th re e -ste p etch-and-rinse
ad hesive system (3M ESPE;
S t Paul, MN, USA)

S cotchbond U niversal E tchant: 32% by

w eigh t phospho ric acid etch in g gel (pH < 1)
P rim er: Ethanol, HEMA, polyalkenoic acid
A dhesive: HEMA, bis-GMA

P rim er: Apply, leave un d istu rb e d fo r 5 s, th e n ge ntly

th in w ith a m ild oil-free a ir stre am fo r 5 s a t a d ista n ce
o f 2 cm fro m d e n tin surface.
A dhesive: Apply, leave u n d istu rb e d fo r 1 5 s, lig h t cure
fo r 1 0 s.

C learfil SE Bond, tw o-com po nen t

tw o-step self-e tc h in g ad hesive
syste m (Kuraray N orita ke; Tokyo,
Japan)

C learfil S3 Bond, one-com pon ent

sin g le -ste p s e lf-e tc h in g ad hesive
syste m (Kuraray N oritake)

P rim er: 10-M DP HEMA, hydrophilic

d im e th a c ry la te , D ,L-cam phorquinone, N,Ndiethano l-p-toluidin e, water.

P rim er: Apply o n to th e visib ly m o is t prepared to o th

surface, leave u n d istu rb e d fo r 2 0 s, th e n dry w ith a
m ild oil-free a ir s tre a m fo r 5 s.

Bond: MDP bis-GMA, HEMA, hydrophobic

dim e thacrylate, dl-cam phorquinone, N,Ndiethanol-p-toluidine, s ilana ted colloidal silica

Bond: Apply one c o a t and a g e n tle oil-free a ir stre am

fo r 5 s, th e n lig h t cure fo r 1 0 s.

MDP bis-GMA, HEMA, water, eth ano l,

hydrophobic d im e th a c ry la te , ph oto-initiator,
s ila n a te d co llo id a l silica

Apply 2 0 s, a ir dry fo r 5 s w ith high-pressure a ir

s tre a m , lig h t cure fo r 1 0 s.

Bis-GMA: bis-phenol-A giycidyl methacrylate; HEMA: 2-hydroxyethyl methacrylate; MDP: methacryloyloxydecyl dihydrogen phosphate.

using a Demetron LED radiom eter (Kerr; Orange, CA,

USA).28 Bonding and resin composite buildup were done
while the tooth segments were subjected to 15 mm Hg
simulated intrapulpal pressure. The specimens were then
immersed in artificial saliva 37 for 24 h at 37C in a spe
cially constructed large incubator to accommodate the in
trapulpal pressure assembly. After 24 h, specimens were
sectioned along the x- and y-axes to obtain multiple sticks
with a cross-sectional area of 0.8 0.01 mm2. From each
specimen, 8 central sticks were selected. The sticks col
lected from each tooth were evenly distributed over the four
study groups (water for 24 h, water with thermocycling, arti
ficial saliva for 24 h, and artificial saliva with thermocy
cling), yielding 28 sticks per group. Thermocycling was done
for 10,000 cycles of 5C to 55C, with a dwell time of 30 s
and a transfer tim e 10 s .56 The artificial saliva was pre
pared as CaCi2 (0.7 m m ol/l), MgCI2 -6H 20 (0.2 m m ol/l),
KH2 P0 4 (4.0 mmol/l), KOI (30 m mol/l), [\laN3 (0.3 mmol/l),
and HEPES buffer (20 m m o l/l ) ].37 Every day, the pH of all
solutions used in the study was checked using a digital pH
m eter (Hanna; Milano, Italy) and the solutions were
changed .50
Microtensile Bond Strength Measurment
Each stick was then fixed to the m icrotensile strength
jjgi3,29 Wjth a cyanoacrylate adhesive (Rocket heavy, Dental
Ventures of America; Corona, CA, USA) and stressed in ten
sion using a universal testing machine (Lloyd Instruments;
Fareham, UK) at a crosshead speed of 0.5 m m /m in until
failure. The tensile force at failure was recorded and con
verted to tensile stress in MPa units using computer soft
ware (Nexygen-MT, Lloyd Instruments). Sticks that failed
before testing were assigned a bond strength of zero MPa
and were included in the statistical analysis .2557 The aver

Vol 18, No 4, 2016

age of the pTBS values for the sticks originating from the
same tooth (two per tooth) was calculated considering the
tooth as a statistical unit .1242
Statistical Analysis
Statistical analysis was performed using multifactor ANOVA
(followed by Bonferronis post-hoc test), in which pTBS was
the dependent variable while the adhesive system type,
storage solution, and storage condition were the indepen
dent variables. The significance of the effect of each inde
pendent variable and its interactions was determined. Stu
dents t-test was used to compare the pTBS values of each
adhesive system with or without thermocyling in each stor
age solution, as well as the pTBS values of each adhesive
system with both storage solutions under each storage con
dition (baseline and thermocycled). p < 0.05 was consid
ered statistically significant. Data were analyzed using
SPSS for Windows (Statistical Package for Social Sciences,
version 15 for MS Windows, SPSS; Chicago, IL, USA).
Failure Mode Analysis
Both fractured sections of each stick (dentin side and resin
composite side) were mounted on an aluminum stub, gold
sputter coated, and observed with a scanning electron mi
croscope (SEM 515, Philips Electronic Instruments; Eind
hoven, The Netherlands) to determine the mode of failure.
The failure mode was classified as: type 1: adhesive failure
at the dentin side; type 2 : cohesive failure in the adhesive
layer; type 3: mixed failure (adhesive failure at the dentin
side/cohesive failure in the adhesive layer); or type 4 :
mixed failure (adhesive failure at the dentin side/cohesive
failure in the adhesive layer/cohesive failure in resin com
posite). The frequency of each mode was expressed in per
cent for each group .31

305

El Deeb et al
Table 2

Mean (SD) microtensile bond strength pTBS in MPa of tested groups

Adhesive system
Adper Scotchbond Multi-Purpose

Clearfil SE Bond

Clearfil S3 Bond

D istilled w ater

A rtificial saliva

D istilled w ater

A rtificial saliva

D istilled w ater

A rtificial saliva

24 h

34.2 (4.5)aA
p tf/tn t = 1 /2 8

33.7 (5.1) aA
p tf/tn t = 0 /2 8

32.7 (6.4) aA
ptf/tn t = 0 /2 8

34.1 (6.1) aA
ptf/tn t = 0 /2 8

29.3 (5.3) aA
p tf/tn t = 0 /2 8

30.1 (4.1) aA
ptf/tn t = 0 /2 8

Thermocycling

16.6 (4.7) aB
ptf/tn t = 3 /2 8

23.5 (7.8) bB
ptf/tn t = 1 /2 8

15.9 (4.3) aB
ptf/tn t = 2 /2 8

24.3 (6.7) bB
ptf/tn t = 2 /2 8

14.9 (4.8) aB
ptf/tn t = 3 /2 8

22.3 (3.6) bB
p tf/tn t = 1 /2 8

p tf/tn t = pre-test faiIure/totaI number of tested sticks. Within rows for each adhesive system, means with different superscript small letters are statistically
significantly different (p < 0.05, t-test); within columns for each adhesive system with each storage solution, means with different superscript capital letters
are statistically significantly different (p < 0.05, t-test).

CL

0)

CD
CO

)
x:
CI

CSE

CD

Distilled water i
Artificial saliva |
Distilled water

Type 1: Adhesive failure at the

dentin side

Artificial saliva

Type 2: Cohesive failure in the

adhesive layer

CN

Distilled water
CO
CO

Artificial saliva
CL

o
>>
o
E
a3
i

CO
CO

CSE

CuO

Type 3: Mixed failure

(adhesive failure at the dentin
side + cohesive failure in the
adhesive layer)

Distilled water
Artificial saliva

Type 4: Mixed failure

(adhesive failure at the dentin
side + cohesive failure in the
adhesive layer + cohesive
failure in resin composite)

Distilled water
Artificial saliva
Distilled water

CO
CO

Artificial saliva
20%

40%

60%

80%

100%

RESULTS
Multifactor ANOVA revealed a significant effect for the stor
age solution (p < 0.01), the storage condition (p < 0.001),
as well as their interaction (p < 0.01). However, no signifi
cant e ffe ct was found for the adhesive system type
(p = 0 .8 3 ) or its interaction with the storage solution
(p = 0.81) and storage condition (p = 0.95) variables. The
interaction among the three variables was not significant
(p = 0.78). The descriptive statistics (means, standard de
viations) are presented in Table 2.
The pTBS values of each adhesive system after 24 h stor
age either in distilled water or artificial saliva were not signifi
cantly different. After thermocycling in both solutions, mean
pTBS values for all tested adhesives significantly decreased
(p < 0.001). Meanwhile, the difference between the pTBS val
ues for all tested adhesives thermocycled in distilled water
and artificial saliva were significantly different (p > 0.01).

306

Fig 2 The percentages of

the recorded modes of fail
ure. SBMP: Adper Scotchbond Multi-Purpose; CSE:
C le a rfil SE Bond; S3:
Clearfil S3 Bond.

Following either 24 h storage or thermocycling in distilled

water, SBMP fractured specimens predominantly showed
failure type 1 (adhesive failure at the dentin side), while
when stored in artificial saliva for 24 h, SBMP specimens
mostly showed failure types 2 (cohesive failure in adhesive
layer) and 3 (mixed failure: adhesive failure at the dentin
side/cohesive failure in the adhesive layer). After thermocy
cling in artificial saliva, failure type 4 (mixed failure: adhe
sive failure at dentin side/cohesive failure in the adhesive
layer/cohesive failure in resin composite) was the most
common mode for SBMP fractured specimens. The CSE
fractured specimens exhibited mostly type 4 failure when
stored for 24 h or thermocycled in either solution. For S3
fractured specimens, type 4 was the predominant mode
after 24 h storage in either solution, whereas type 3 was
frequently recorded after thermocycling in either solution.
Figure 2 shows the percentages of failure modes of all
tested groups.

The Journal of Adhesive Dentistry

El Deeb et al

DISCUSSION
The present study findings revealed that the use of different
storage solutions for 24 h had no influence on the microtensile bond strength of the tested adhesives; thus, the
first null hypothesis failed to be rejected. However, because
the pTBS values of all tested adhesives decreased signifi
cantly after thermocyling, the second null hypothesis should
be rejected. The third null hypothesis m ust also be re
jected, as there was a significant difference between the
microtensile bond strengths of the thermocycled adhesives
in distilled water and those in artificial saliva.
As presented, the baseline results did not predict the
future behavior of the tested adhesive systems; a dramatic
decrease in the microtensile bond strength of the dentin
adhesives was associated with therm ocycling in both
media. The commonly observed reduction in bond strength
could be partially attributed to the chemical degradation of
both collagen fib rils and resinous polymers by hydroly
sis. 2-3'1147,18,20 Moreover, the high thermal contraction/
expansion coefficient of the adhesives compared to tooth
tissue generates repeated interfacial contraction/expansion
stresses that could be similar to those in the oral cavity,
which may eventually result in crack propagation along the
resin/dentin interface.
Because the degree of hydrolysis depends on the
amount of reactive ions and their degree of diffusion,46-51
the difference between the water results (48% to 50% de
crease in bond strength) and the artificial saliva results
(26% to 30% decrease in bond strength) could be explained
on the basis of their differences in hydrolytic degradation
potential. To date, no published data on the effect of these
storage media (artificial saliva vs distilled water) on dentin
adhesive bond strength is available. According to Ficks first
law of diffusion,5 the higher the concentration difference of
a certain particle is, the higher is its flux (ie, its permeation
through the dentin/adhesive interface in this case). The
concentration of water molecules is higher in distilled water
than in saliva. This leads to higher diffusion of water mole
cules through the dentin/adhesive interface when stored in
water than in artificial saliva. A study comparing the leachability of resin composite components when stored in dis
tilled water or artificial saliva revealed a significant differ
ence between the leached components in the two storage
solutions, as well as interaction between storage solution
and resin composite constituents.51 Bauer and llie4 found
that aging in artificial saliva rather than distilled water im
proved the micromechanical properties of resin composites.
Additionally, it has been reported that the glass-ionomer
restorative materials possessed higher surface hardness
when stored in human saliva compared to distilled water.34
Based on the previous and the current findings, it seems
that the use of distilled water as a storage solution de
creases the similarity of in vitro studies to the clinical find
ings.
In addition to diffusion-dependent hydrolysis, thermocy
cling causes repetitive contraction/expansion stress. Diffu
sion-dependent hydrolysis caused by hot water may acceler

Vol 18, No 4, 2016

ate the hydrolysis of unprotected collagen and extract

poorly polymerized resin oligom ers.18-27 Moreover, the
three adhesive systems contain HEMA. HEMA is a hydro
philic monomer which imbibes a large amount of water
within the adhesive and the hybrid layer53 during thermocy
cling. Hence, water remains entrapped at the resin/dentin
interface, causing swelling and plasticization of the poly
mers, which results in reduction of their mechanical proper
ties.58
The significant reduction of bond strength of the etchand-rinse adhesive system (SBMP) following thermocycling
could be related to the discrepancies between the extent of
demineralization and the depth of infiltration of the adhe
sive resin. Such a mismatch has been claimed to affect the
stability of the resin-dentin bond, as hydrolysis of the colla
gen peptides may occur and weaken the adhesive joint over
tim e .6-45-49 The degradation of incompletely infiltrated
zones within the hybridized dentin may continue even in the
absence of bacterial enzymes.37 The significant reduction
of bond strength o f the SBMP adhesive system after
3 months storage in distilled water has been reported by
others.49
The bond strength reduction with the two-step self-etch
ing adhesive (CSE) might be explained by both the hydro
lytic degradation of polymers occurring after water sorption
and the permeability of the adhesive layer,9 especially as
the four sides of the cut sticks in the present study were
exposed to the storage solution, rather than being exposed
as a whole, uncut specimen. CSE contains hydrophilic
monomers, prone to water sorption over time, which could
contribute to the observed reduction in bond strength. This
is despite the fact that CSE contains 10-MDP, which the
literature1-19-41 - including a recent clinical study38 - has
reported to provide bond stability.
The reduction in bond strength of S3 following thermocy
cling could be due to the behavior of bonded interfaces as
semi-permeable membranes.40-45 Being highly hydrophilic,
it is very difficult to remove water from the adhesive resin of
one-step self-etching adhesives, which could jeopardize its
polymerization efficacy and in turn lower its mechanical
properties.44-52 Recently, it has been shown that MMP acti
vation is induced by dentin adhesives, irrespective of the
strategy employed (ie, etch-and-rinse or self-etching).26
These endogenous gelatinolytic/collagenolytic enzymes can
degrade the collagen structure of the bonded interface over
tim e, accelerating the degradation of the adhesive inter
face.23 Nevertheless, whether the MMP types activated and
their activation rates would differ based on the storage me
dium used (distilled water and artificial saliva) still requires
investigation. It must also be borne in mind that application
of simulated intrapulpal pressure during bonding increases
convective fluid movement and leads to the formation of
water channels through the polymerized adhesives.47
Although distilled water was more aggressive as an
aging medium, it cannot be considered as the appropriate
means of testing the real performance of the adhesive res
toration during clinical service. On the other hand, it is well
known that duplicating the exact properties of human saliva

307

El Deeb et a I
is nearly impossible due to its inconsistency and instability.
This in turn m akes natural saliva inappropriate fo r use in
standardized long-term in vitro stu d ie s.21 Despite th is lim i
tation, the developm ent o f artificial saliva is essential for
well-justified and controlled experiments. It provides a sta
ble electrolytic com position with a constant pH (7) com pat
ible with the standardized m ethods o f aging. Nevertheless,
te s tin g in com parable experim ental in vivo co nditions re
m ains necessary to a ssess the bonding performance and
durability o f the restorations.

17. Giannini M, Seixas CA, Reis AF, Pimenta LA. Six-month storage-time
evaluation of one-bottle adhesive systems to dentin. J Esthet Restor
Dent 2003;15:43-49.
18. Hashimoto M, Ohno H, Kaga M, Endo K, Sano H, Oguchi H. In vivo degra
dation of resin-dentin bonds in humans over 1 to 3 years. J Dent Res
2000;79:1385-1391.
19. Inoue S, Koshiro K, Yoshida Y, De Munck J, Nagakane K, Suzuki K,
Sano H, Van Meerbeek B. Hydrolytic stability of self-etch adhesives
bonded to dentin. J Dent Res 2005;84:1160-1164.
20. Kitasako Y, Burrow MF, Nikaido T, Tagami J. The influence of storage so
lution on dentin bond durability of resin cement. Dent Mater 2000;16:

1-6 .
21. Leung VW, Darvell BW. Artificial salivas for in vitro studies of dental ma
terials. J Dent 1997;25:475-484.

CONCLUSION

22. Manso AP, Marquezini L Jr, Silva SM, Pashley DH, Tay FR, Carvalho RM.
Stability of wet versus dry bonding with different solvent-based adhe
sives. Dent Mater 2008;24:476-482.

The decrease in bond strength was more pronounced for

specim ens stored in distilled water than in artificial saliva.

23. Marchesi G, Frassetto A, Mazzoni A, Apolonio F, Diolosa M, Cadenaro M,

Di Lenarda R, Pashley DH, Tay F, Breschi L. Adhesive performance of a
multi-mode adhesive system: 1-year in vitro study. J Dent 2014;42:
603-612.

REFERENCES
1.

2.

Anchieta RB, Machado LS, Martini AP, Santos PH, Giannini M, Janal M,
Tovar N, Sundfeld RH, Rocha EP, Coelho PG. Effect of long-term storage
on nanomechanical and morphological properties of dentin-adhesive in
terfaces. Dent Mater 2015;31:141-153.
Armstrong SR, Keller JC, Boyer DB. The influence of water storage and cfactor on the dentin-resin composite microtensile bond strength and
debond pathway utilizing a filled and unfilled adhesive resin. Dent Mater
2001;17:268-276.

3.

Armstrong SR, Vargas MA, Fang Q, Laffoon JE. M icrotensile bond

strength of a total-etch 3-step, total-etch 2-step, self-etch 2-step, and a
self-etching 1-step dentin bonding system through 15-month water stor
age. J Adhes Dent 2003;5:47-56.

4.

Bauer H, Hie N. Effects of aging and irradiation time on the properties of

a highly translucent resin-based composite. Dent Mater J 2013;32:
592-599.

5.

Bird RB, Stewart WE, Lightfoot EN. Transport phenomena, ed 10. Hobo
ken, NJ: John Wiley & Sons, 2002.

6.

Breschi L, Cammelli F, Visintini E, Mazzoni A, Vita F, Carrilho M, Cadenaro M, Foulger S, Mazzoti G, Tay FR, Di Lenarda R, Pashley D. Influence
of chlorhexidine concentration on the durability of etch-and-rinse dentin
bonds: A 12-month in vitro study. J Adhes Dent 2009;11:191-198.

7.

8.

9.

Breschi L, Mazzoni A, Nato F, Carrilho M, Visintini E, Tjaderhane L, Ruggeri A Jr, Tay FR, Dorigo Ede S, Pashley DH. Chlorhexidine stabilizes the
adhesive interface: A 2-year in vitro study. Dent Mater 2010;26:320-325.
Carrilho MR, Carvalho RM, De Goes MF, Di Hipolito V, Geraldeli S,
Tay FR, Pashley DH, Tjaderhane L. Chlorhexidine preserves dentin bond
in vitro. J Dent Res 2007;86:90-94.
Da Silva Nunes Gomes Miranda ME, De Oliveira Scudine KG, Noronha
Filho JD, Moreira Da Silva E, Amaral CM. Sorption and solubility of self
etching adhesives immersed in organic acids present in oral biofilm.
J Adhes Dent 2014;16:115-122.

10. De Munck J, Van Landuyt K, Peumans M, Poitevin A, Lambrechts P,

Braem M. Van Meerbeek B. A critical review of the durability of adhesion
to tooth tissue: Methods and results. J Dent Res 2005;84:118-132.
11. De Munck J, Van Meerbeek B, Yoshida Y, Inoue S, Vargas M, Suzuki K,
Lambrechts P, Vanherle G. Four-year water degradation of total-etch ad
hesives bonded to dentin. J Dent Res 2003;82:136-140.
12. Eckert GJ, Platt JA. A statistical evaluation of microtensile bond strength
methodology for dental adhesives. Dent Mater 2007;23:385-391.
13. El Zohairy AA, De Gee AJ, De Jager N, Van Ruijven U , Feilzer AJ. The in
fluence of specimen attachment and dimension on microtensile strength.
J Dent Res 2004;83:420-424.
14. Frankenberger R, Strobel WO, Lohbauer U, Kramer N, Petschelt A. The ef
fect of six years of water storage on resin composite bonding to human
dentin. J Biomed Mater Res B Appl Biomater 2004;69:25-32.
15. Fukegawa D, Hayakawa S, Yoshida Y, Suzuki K, Osaka A, Van Meer
beek B. Chemical interaction of phosphoric acid ester with hydroxyapa
tite. J Dent Res 2006;85:941-944.
16. Gale MS, Darvell BW. Thermal cycling procedures for laboratory testing of
dental restorations. J Dent 1999;27:89-99.

308

24. Marchesi G, Frassetto A, Visintini E, Diolosa M, Turco G, Salgarello S, Di

Lenarda R, Cadenaro M, Breschi L. Influence of ageing on self-etch adhe
sives: One-step vs. Two-step systems. Eur J Oral Sci 2013;121:43-49.
25. Mazzitelli C, Monticelli F, Osorio R, Casucci A, Toledano M, Ferrari M. Ef
fect of simulated pulpal pressure on self-adhesive cements bonding to
dentin. Dent Mater 2008;24:1156-1163.
26. Mazzoni A, Scaffa P, Carrilho M, Tjaderhane L, Di Lenarda R, Polimeni A,
Tezvergil-Mutluay A, Tay FR, Pashley DH, Breschi L. Effects of etch-andrinse and self-etch adhesives on dentin mmp-2 and mmp-9. J Dent Res
2013;92:82-86.
27. Miyazaki M, Sato M, Onose H, Moore BK. Influence of thermal cycling on
dentin bond strength o f tw o-step bonding system s. Am J Dent
1998;11:118-122.
28. Mobarak E, El-Deeb H. Two-year interfacial bond durability and nanoleak
age of repaired silorane-based resin composite. Oper Dent 2013;38:
408-418.
29. Mobarak E, El-Deeb H, El-Samman M. The difference in microtensile-bond
strength jigs influences the test outcome. J Dent Res 2013:92:69.
30. Mobarak EH. Effect of chlorhexidine pretreatment on bond strength dura
bility of caries-affected dentin over 2-year aging in artificial saliva and
under simulated intrapulpal pressure. Oper Dent 2011;36:649-660.
31. Mobarak EH, El-Badrawy W, Pashley DH, Jamjoom H. Effect of pretest
storage conditions of extracted teeth on their dentin bond strengths.
J Prosthet Dent 2010;104:92-97.
32. Mobarak EH, El-Badrawy WH. Microshear bond strength of self-etching
adhesives to caries-affected dentin identified using the dye permeability
test. J Adhes Dent 2012;14:245-250.
33. Mobarak EH, El-Korashy DI, Pashley DH. Effect of chlorhexidine concen
trations on micro-shear bond strength of self-etch adhesive to normal and
caries-affected dentin. Am J Dent 2010;23:217-222.
34. Okada K, Tosaki S, Hirota K, Hume WR. Surface hardness change of re
storative filling materials stored in saliva. Dent Mater 2001;17:34-39.
35. Okuda M, Pereira PN, Nakajima M, Tagami J. Relationship between
nanoleakage and long-term du rability o f dentin bonds. Oper Dent
2001;26:482-490.
36. Okuda M, Pereira PN, Nakajima M, Tagami J, Pashley DH. Long-term du
rability of resin dentin interface: nanoleakage vs m icrotensile bond
strength. Oper Dent 2002;27:289-296.
37. Pashley DH, Tay FR, Yiu C, Hashimoto M, Breschi L, Carvalho RM, Ito S.
Collagen degradation by host-derived enzymes during aging. J Dent Res
2004;83:216-221.
38. Peumans M, De Munck J, Van Landuyt K, Van Meerbeek B. Thirteen-year
randomized controlled clinical trial of a two-step self-etch adhesive in
non-carious cervical lesions. Dent Mater 2015;31:308-314.
39. Pimenta LA, Amaral CM, Bedran De Castro AK, Ritter AV. Stability of den
tin bond strengths using different bonding techniques after 12 months:
Total-etch, deproteinization and self-etching. Oper Dent 2 0 0 4 ;2 9 :
592-598.
40. Reis A, Grandi V, Carlotto L, Bortoli G, Patzlaff R, Rodrigues Accorinte
Mde L, Dourado Loguercio A. Effect of smear layer thickness and acidity
of self-etching solutions on early and long-term bond strength to dentin.
J Dent 2005;33:549-559.
41. Reis AF, Giannini M, Pereira PN. Long-term tern analysis of the nanoleak
age patterns in resin-dentin interfaces produced by different bonding
strategies. Dent Mater 2007;23:1164-1172.

The Journal of Adhesive Dentistry

El Deeb et al
42. Roulet JF, Van Meerbeek B. Statistics: A nuisance, a tool, or a must?
J Adhes Dent 2007;9:287-288.
43. Sadek FT, Castellan CS, Braga RR, Mai S, Tjaderhane L, Pashley DH,
Tay FR. One-year stability of resin-dentin bonds created with a hydropho
bic ethanol-wet bonding technique. Dent Mater 2010;26:380-386.
44. Sadr A, Shimada Y, Tagami J. Effects of solvent drying time on micro
shear bond strength and mechanical properties of two self-etching adhe
sive systems. Dent Mater 2007;23:1114-1119.

55. Turssi CP, Hara AT, Serra MC, Rodrigues AL Jr. Effect of storage media
upon the surface micromorphology of resin-based restorative materials.
J Oral Rehabil 2002;29:864-871.
56. Ulker M, Ozcan M, Sengun A, Ozer F, Belli S. Effect of artificial aging regi
mens on the performance of self-etching adhesives. J Biomed Mater Res
B Appl Biomater 2010;93:175-184.

45. Salz U, Zimmermann J, Zeuner F, Moszner N. Hydrolytic stability of self

etching adhesive systems. J Adhes Dent 2005;7:107-116.

57. Van Landuyt KL, Mine A, De Munck J, Jaecques S, Peumans M, Lambrechts P, Van Meerbeek B. Are one-step adhesives easier to use and
better performing? Multifactorial assessment of contemporary one-step
self-etching adhesives. J Adhes Dent 2009;11:175-190.

46. Sano H, Yoshikawa T, Pereira PN, Kanemura N, Morigami M, Tagami J,

Pashley DH. Long-term durability of dentin bonds made with a self-etching
primer, in vivo. J Dent Res 1999;78:906-911.

58. Van Landuyt KL, Snauwaert J, De Munck J, Coutinho E, Poitevin A, Yoshida Y, Suzuki K, Lambrechts P, Van Meerbeek B. Origin of interfacial
droplets with one-step adhesives. J Dent Res 2007;86:739-744.

47. Sauro S, Pashley DH, Montanari M, Chersoni S, Carvalho RM, Toledano M, Osorio R, Tay FR, Prati C. Effect of simulated pulpal pressure on
dentin permeability and adhesion of self-etch adhesives. Dent Mater
2007;23:705-713.

59. Van Meerbeek B, De Munck J, Yoshida Y, Inoue S, Vargas M, Vijay P, Van

Landuyt K, Lambrechts P, Vanherle G. Buonocore memorial lecture. Adhe
sion to enamel and dentin: Current status and future challenges. Oper
Dent 2003;28:215-235.

48. Sengun A, Ozturk B, Ozer F. The effect of simulated intrapulpal pressure

on bond strength to enamel and dentine. J Oral Rehabil 20 03;3 0:
550-555.

60. Yamazaki PC, Bedran-Russo AK, Pereira PN. Importance of the hybrid
layer on the bond strength of restorations subjected to cyclic loading.
J Biomed Mater Res B Appl Biomater 2008;84:291-297.

49. Shinohara MS, De Goes MF, Schneider LF, Ferracane JL, Pereira PN, Di
Hipolito V, Nikaido T. Fluoride-containing adhesive: Durability on dentin
bonding. Dent Mater 2009;25:1383-1391.

61. Yoshida Y, Nagakane K, Fukuda R, Nakayama Y, Okazaki M, Shintani H,

Inoue S, Tagawa Y, Suzuki K, De Munck J, Van Meerbeek B. Comparative
study on adhesive performance of functional monomers. J Dent Res
2004;83:454-458.

50. Skovron L, Kogeo D, Gordillo LA, Meier MM, Gomes OM, Reis A, Loguercio AD. Effects of immersion time and frequency of water exchange on
durability of etch-and-rinse adhesive. J Biomed Mater Res B Appl Bioma
ter 2010;95:339-346.
51. Soderholm KJ, Mukherjee R, Longmate J. Filler leachability of composites
stored in d is tille d water or a rtificia l saliva. J Dent Res 1 9 9 6 ;7 5 :
1692-1699.
52. Spreafico D, Semeraro S, Mezzanzanica D, Re D, Gagliani M, Tanaka T,
Sano H, Sidhu SK. The effect of the air-blowing step on the technique
sensitivity of four different adhesive systems. J Dent 2006;34:237-244.
53. Tay FR, Pashley DH, Suh Bl, Carvalho RM, Itthagarun A. Single-step adhe
sives are permeable membranes. J Dent 2002;30:371-382.
54. Toledano M, Osorio R, Osorio E, Aguilera FS, Yamauti M, Pashley DH,
Tay F. Effect of bacterial collagenase on resin-dentin bonds degradation.
J Mater Sci Mater Med 2007;18:2355-2361.

Vol 18, No 4, 2016

Clincal relevance: The present study showed a differ

ence in the effect of artificial saliva and distilled water

on adhesive systems bond durability, which may help
make in vitro studies more comparable to the clinical
situation and bridge the gap between the outcome of in
vitro studies and clinical trials.

309

Copyright of Journal of Adhesive Dentistry is the property of Quintessence Publishing

Company Inc. and its content may not be copied or emailed to multiple sites or posted to a
listserv without the copyright holder's express written permission. However, users may print,
download, or email articles for individual use.