Dry-bonding Etch-and-Rinse Strategy Improves Bond

Longevity of a Universal Adhesive to Sound and

Artificially-induced Caries-affected Primary Dentin
Tathiane Larissa Lenzia / Fabio Zovico Maxnuck Soaresb / Daniela Prócida Raggioc /
Gabriel Kalil Rocha Pereirad / Rachel de Oliveira Rochae

Purpose: To evaluate the effect of the etching strategy on the immediate and 1-year microtensile bond strength
(μTBS) and structural reliability of a universal adhesive to sound and artificially-induced caries-affected dentin of pri-
mary teeth.
Materials and Methods: Flat midcoronal dentin surfaces were exposed in 50 primary molars, which were then ran-
domly assigned to 10 groups according to substrate (sound dentin [SD] and artificially-induced caries-affected den-
tin [CAD] with pH cycling for 14 days) and etching approach using Scotchbond Universal Adhesive (self-etching or
dry or wet-bonding etch-and-rinse strategies) with Adper Single Bond Plus (two-step etch-and-rinse adhesive) and
Clearfil SE Bond (two-step self-etching system) as controls. Composite buildups were constructed and sectioned to
obtain bonded sticks (0.8 mm2) to be subjected to microtensile testing immediately or after 1 year of water aging.
Data were analyzed using three-way repeated measures ANOVA and Tukey’s test (α = 0.05). Weibull modulus and
characteristic strength were also determined.
Results: A decrease in bond strength was observed after 1 year of water aging, except when the universal adhe-
sive was used in the dry-bonding etch-and-rinse and self-etching approaches. However, the self-etching approach
resulted in lower μTBS values in SD, while no difference among experimental groups was observed in CAD. Overall,
higher Weibull modulus values were achieved in the groups with higher bond strength. The relationship between
characteristic strength and bond strengths was not linear for all groups.
Conclusion: The bond longevity of the universal adhesive using the dry-bonding etch-and-rinse approach on sound
and artificially-induced caries-affected primary dentin was better than the other bonding agents and approaches
tested.
Keywords: multimode adhesive, structural reliability, caries-affected dentin, deciduous tooth, durability, microtensile.

J Adhes Dent 2016; 18: 475–482. Submitted for publication: 17.12.15; accepted for publication: 30.07.16
doi: 10.3290/j.jad.a36670

A novel category of one-bottle adhesives, termed universal

or multimode adhesives, has recently been proposed to
be used following either an etch-and-rinse or self-etching
a Professor, Graduate Program in Dental Science, Federal University of Santa
Maria, Brazil. Performed the experiments, wrote the manuscript.
b Professor, Department of Restorative Dentistry, Federal University of Santa
Maria, Brazil. Contributed substantially to discussion, proofread the manu-
script.
c Associate Professor, Department of Pediatric, Dentistry, School of Dentistry,
University of São Paulo, São Paulo, SP, Brazil. Contributed substantially to dis-
cussion, proofread the manuscript.
d PhD Student, Graduate Program in Dental Science, Federal University of
Santa Maria, Brazil. Consulted on and performed statistical evaluation, proof-
read the manuscript.
e Associate Professor, Department of Stomatology, Federal University of Santa
Maria, Brazil. Idea, experimental design, proofread the manuscript.
Correspondence: Rachel de Oliveira Rocha, Department of Stomatology,
Federal University of Santa Maria, Rua Marechal Floriano Peixoto, 1184,
97015-270, Santa Maria, RS, Brazil. Tel: +55-55-3220-9266;
e-mail: rachelrocha@smail.ufsm.br
strategy, with the intent of making the clinical procedure
more user friendly. Further, the universal adhesives can be
applied on dry or wet demineralized dentin, reducing the
possibility of iatrogenically induced misapplication during
acid conditioning, rinsing and drying, which may occur when
using etch-and-rinse systems.4
Which adhesive protocol is best for universal adhesives
still cannot be indisputably determined, based on the
scarce and ambiguous evidence available, mainly with re-
gard to the stability of resin-dentin bonds created by these
adhesives.16,18 Interestingly, the manufacturers also claim
that their use does not rely upon the dental substrate being
prepared for restoration. The main challenge for current ad-
hesives has been to provide equally effective performance
on dental substrates of different natures.18,21 From a clin-
ical point of view, these bonding substrates are mostly
caries-affected dentin (CAD) rather than sound dentin.
Bonding to CAD is notoriously critical,10,12,27 using either
self-etching or etch-and-rinse adhesives. Considering the

Vol 18, No 6, 2016 475

Lenzi et al
“universal application” idea, it might be expected that the
efficacy of new one-bottle adhesives is not influenced by the
substrate condition. Nevertheless, the performance of the
universal adhesives on different substrates, such as CAD, is
poorly investigated.14 To the best of our knowledge, the cur-
rent study is the first to examine whether a universal adhe-
sive system can be applied in a multimode manner, following
either a self-etching or dry- or wet-bonding etch-and-rinse ap-
proach, without jeopardizing the resin-CAD bonds over time.
Although clinical trials with longer follow-up periods pro-
vide more useful information for clinical evidence-based deci-
sion-making, laboratory studies are necessary for testing new
materials or protocols. Bond strength results usually vary
highly5 as a consequence of the interaction of brittle mater-
ials with superficially demineralized dentin. In this sense,
Weibull statistics has been used to assess the structural
reliability of the adhesive interface,5,28 providing an estimate
of failure probability of dental materials. Therefore, the pur-
pose of this study was to investigate the influence of the
etching strategy on the immediate and 1-year microtensile
bond strength (μTBS) and structural reliability of a universal
adhesive to sound and artificially-induced caries-affected den-
tin of primary teeth. The null hypothesis tested was that the
immediate and 1-year bond strength and structural reliability
of a universal adhesive are not influenced by the etching
strategy selected, irrespective of the substrate.
MATERIALS AND METHODS
Tooth Selection and Preparation
After approval from the Institutional Ethics Board, 50 sound
second primary molars were selected from the human tooth
bank of the University.3 The teeth were disinfected in 0.5%
aqueous chloramine, and stored in distilled water at 4°C
until use. The occlusal enamel was removed with a water-
cooled diamond saw in a cutting machine (Labcut 1010,
Extec; Enfield, CT, USA) to obtain flat midcoronal dentin
surfaces. The surrounding enamel was also removed with a
diamond bur in a high-speed handpiece (# 3195, KG So-
rensen; Barueri, Brazil) with water spray. The dentin sur-
faces were carefully examined under a stereomicroscope at
30X magnification to confirm the absence of enamel islets.
The exposed dentin surfaces were further polished with
600-grit silicon carbide abrasive paper under running water
for 30 s to obtain a uniform, standardized smear layer.
Artificial Caries Induction
Specimens were randomly allocated into two groups which
underwent different procedures: 1. immersion in distilled
water at 37°C during the experimental period, no pH cycling
(control group; sound dentin [SD]); 2. exposure to artificial
caries induction with a pH-cycling model (experimental
group; artificially-induced caries-affected dentin [CAD]). The
cervical portions of the teeth were sealed with epoxy resin
(Araldite Hobby, Ciba Especialidades Químicas; São Paulo,
SP, Brazil) and received two layers of acid-resistant nail pol-
ish (Colorama Maybelline; São Paulo, SP, Brazil). Then,
476
specimens were individually immersed in 10 ml of deminer-
alizing solution (2.2 mM CaCl2, 2.2 mM NaH2PO4, 50 mM
acetic acid, adjusted pH of 4.8) for 8 h and in the same
volume of remineralizing solution (1.5 mM CaCl2, 0.9 mM
NaH2PO4, 0.15 mM KCl, adjusted pH of 7.0) for 16 h. This
procedure was carried out for 14 days at room temperature
without agitation. The solutions were renewed at each
cycle.13
Experimental Design
Teeth from each dentin substrate (SD or CAD) were randomly
reassigned to five subgroups according to the different bond-
ing strategies of the selected adhesive systems. Scotchbond
Universal Adhesive (3M ESPE; St Paul, MN, USA) was ap-
plied on dentin surfaces using either a self-etching or a dry-
or wet-bonding etch-and-rinse adhesive protocol. As controls,
the two-step etch-and-rinse adhesive Adper Single Bond Plus
(3M ESPE) and two-step self-etching adhesive Clearfil SE
Bond (Kuraray Noritake; Tokyo, Japan) were used. A total of
ten experimental conditions were tested in this study, and
n = 5 teeth were randomly assigned to each group.
Bonding Procedures and Specimen Preparation
The adhesive systems were applied according to the manu-
facturer’s instructions (Table 1). After the bonding proced-
ures, a resin composite (Filtek Z250, shade A1, 3M ESPE)
was placed in two increments of 2 mm each on dentin
surfaces, and each increment was light cured for 20 s with a
light-emitting diode curing unit (Emitter B, Schuster; Santa
Maria, RS, Brazil) at a light output of at least 1250 mW/cm2.
Light output was monitored with a Demetron Curing Radiom-
eter (Kerr; Orange, CA, USA). A single trained operator car-
ried out all procedures. After 24 h of water storage, speci-
mens were sectioned longitudinally in the mesiodistal and
buccolingual directions across the bonded interface with a
water-cooled diamond saw in a cutting machine (Labcut
1010, Extec), obtaining sticks with a cross-sectional area of
approximately 0.8 mm2. The cross-sectional area of each
stick was measured with a digital caliper (Absolute Digimatic,
Mitutoyo; Tokyo, Japan) to calculate the bond strengths in
MPa. The sticks were carefully examined with a stereomicro-
scope at 30X magnification, and those with defects at the
resin/dentin interface were discarded.
Microtensile Bond Strength (μTBS) Testing
Bonded sticks originating from the same teeth were ran-
domly subdivided according to the storage period, 24 h or
1 year in distilled water at 37°C. The storage solution was
not changed and its pH was monitored monthly. After each
storage period, the bonded sticks were attached with
cyanoacrylate resin to a device for microtensile testing and
subjected to microtensile testing in a universal testing ma-
chine (Emic; São José dos Pinhais, PR, Brazil) at a cross-
head speed of 1 mm/min.
Failure Mode
A single observer evaluated all debonded specimens under
a stereomicroscope (HMV II, Shimadzu; Kyoto, Japan) at
The Journal of Adhesive Dentistry
 Lenzi et al

Table 1 Composition and application mode of the adhesive system tested

Adhesive system Main components pH* Self-etching strategy Etch-and-rinse strategy

Scotchbond Universal Etchant: 34% phosphoric acid,
Adhesive water, synthetic amorphous silica,
(3M ESPE; St Paul, MN, polyethylene glycol, aluminum
USA) oxide
MDP phosphate monomer,
dimethacrylate resins, HEMA,
methacrylate-modified polyalkenoic
acid copolymer, filler, ethanol,
water, initiators, silane
0.1 1. Keep dentin dry, do not
overdry.
2. Apply the adhesive for 20 s
with vigorous agitation.
6. Gently air thin for 5 s.
2.7 7. Light cure for 10 s.
1. Apply etchant for 15 s.
2. Rinse for 10 s.
3. Air dry to remove excess
water.
4. Keep dentin moist
(wet-bonding approach) or
keep dentin dry, do not
overdry (dry-bonding
approach).
5. Apply the adhesive as for
the self-etching mode.

Adper Single Bond Plus
(3M ESPE)
Etchant: 35% phosphoric acid 0.6 1. Apply etchant for 15 s.
2. Rinse for 10 s.
HEMA, water, ethanol, bis-GMA, 4.7 N. A. 3. Blot excess water.
dimethacrylates, amines, 4. Apply 2 consecutive coats
methacrylate-functional copolymer of adhesive for 15 s with
of polyacrylic and polyitaconic gentle agitation.
acids, 10% by weight of 5 5. Gently air dry for 5 s.
nanometer-diameter spherical 6. Lightcure for 10 s.
silica particles

Clearfil SE Bond
(Kuraray Noritake; Tokyo,
Japan)
Primer: MDP, HEMA, hydrophilic
dimethacrylate, dl-camphorquinone,
N,N-diethanol-p-toluidine, water
Bonding: MDP, bis-GMA, HEMA,
hydrophobic dimethacrylate, dl-
camphorquinone, N,N-diethanol-p-
toluidine, silanated colloidal silica
2.0 1. Apply primer on dry dentin
surface and leave
undisturbed for 20 s.
2. Dry with air stream for 5 s to
evaporate the volatile
ingredients. N. A.
3. Apply bond and gently air dry.
4. Light cure for 10 s.

MDP: 10-methacryloyloxydecyl-dihydrogen-phosphate; bis-GMA: bisphenyl-glycidyl methacrylate; HEMA: 2-hydroxyethyl methacrylate. *pH values were provided
by the manufacturers. N. A.: not applicable.

400X magnification to determine the failure mode: interfa-
cial (failure at the resin/dentin interface) or cohesive (fail-
ure exclusively within the dentin or resin composite).
Statistical Analysis
The experimental unit in the current study was the tooth.
Half the specimens of each tooth were tested after 24 h
of water storage and the other half after 1 year. Thus, the
mean μTBS (MPa) of all sticks from the same hemi-tooth
was averaged for statistical purposes. The mean μTBS for
every tested group was expressed as the average of five
hemi-teeth per group. The number of prematurely
debonded sticks in each group was recorded, but pre-test
failures were not included in the statistical analysis. Spec-
imens with cohesive failures were also excluded from the
data analysis. Failure modes were analyzed descriptively.
Normal distribution of the data was confirmed using the
Kolmogorov-Smirnov test. The μTBS means were analyzed
using three-way ANOVA (substrate vs etching strategy vs
storage period) and Tukey’s post-hoc test at α = 0.05 for
pairwise comparisons. The clustered variable was the stor-
age period. Weibull statistical analysis was used to deter-
mine the probability of failure depending on adhesive bond
strength. The probability Pf that the specimen fails at
stress σ is defined as follows: Pf = 1 - exp [–(σ/σo)m],
where the scale parameter or the characteristic strength,
σ, is the bond strength at which 63.2% of the samples fail
and is thus a measure of adhesive bond strength. Weibull
modulus, m, or the shape parameter, reflects the distribu-
tion of fracture-initiating flaws. High values of m indicate a
narrow distribution of defects and more predictable failure
behavior, while low m is typical for a high spread of de-
fects and less predictable bond strength. The m param-
eter is thus a measure of bond strength variability. Proba-
bility of failure at a given stress can be calculated as
Pf = i/(N+1) where i is its rank number in the ascending
order of bond strength data of N samples. The parameters
of Weibull distribution can be obtained from the slope and
intercept of ln [ln(1-Pf)] vs ln σ data. Using characteristic
strength and the Weibull modulus, the bond strength at a
selected probability of failure can be calculated and used
to characterize the structural reliability of adhesive sys-
tems. The Weibull distribution parameters were calculated
using the maximum likelihood estimation method at a 95%
confidence level.
RESULTS
The main factors “etching strategy” (p < 0.001), “sub-
strate” (p < 0.001), and “storage period” (p < 0.001) as
well as the cross-product interactions, “etching strategy vs
substrate” (p < 0.001) and “etching strategy vs storage pe-
riod” (p = 0.021) were statistically significant (Table 2).
In SD, the universal adhesive applied using both dry- and
wet-bonding etch-and-rinse strategies showed higher bond

Vol 18, No 6, 2016 477

Lenzi et al

Table 2 Microtensile bond strength in MPa (means ± SD) considering the cross-product interactions “etching time
vs substrate” and “etching time vs storage period”

Substrate Storage period

Etching strategy Sound dentin Caries-affected dentin 24 h 1 year

Scotchbond Universal Adhesive 43.0 ( 10.1a 21.2 ( 6.4d 36.9 ( 15.1A 27.3 ( 11.3B,C,D
Wet-bonding etch-and-rinse

Scotchbond Universal Adhesive 41.9 ( 7.9a,b 21.4 ( 7.0d 35.6 ( 13.3A,B 27.7 ( 11.4B,C
Dry-bonding etch-and-rinse

Scotchbond Universal Adhesive 26.2 ( 6.2c,d 19.6 ( 5.3d 24.5 ( 6.1C,D 21.3 ( 6.8C,D
Self-etching

Adper Single Bond Plus 34.3 ( 11.6b,c 19.6 ( 8.5d 35.0 ( 10.9A,B 18.9 ( 8.0D
Etch-and-rinse control

Clearfil SE Bond 41.7 ( 5.5a,b 17.9 ( 7.7d 34.3 ( 11.5A,B 25.3 ( 15.0C,D
Self-etching control

Different superscript capital letters indicate significant differences considering the cross-product interaction “etching strategy vs storage period”. Different su-
perscript lower case letters indicate statistically significant for the cross-product interaction “etching strategy vs substrate” (p < 0.05).

strengths in comparison with the self-etching mode, which
in turn also presented lower μTBS than those obtained with
the control self-etching adhesive. Moreover, the universal
adhesive applied in wet-bonding etch-and-rinse mode pro-
moted better adhesive performance than did the control
etch-and-rinse adhesive.
The μTBS values obtained for CAD were significantly
lower than those obtained for SD, except when the univer-
sal adhesive was applied in the self-etching mode. No dif-
ference among adhesives and etching strategies was ob-
served when their performances were compared in
caries-affected dentin.
One year of water storage resulted in a significant reduc-
tion in bond strength, except when the universal adhesive
was used in the dry-bonding etch-and-rinse and self-etching
approaches, irrespective of the dentin condition.
Microtensile bond strengths, Weibull modulus, charac-
teristic strength and respective confidence intervals for
all experimental conditions are presented in Table 3. In
general, a lower m was observed in CAD than in SD, indi-
cating a wider scatter of the results, and consequently, a
lower reliability of bonding to this substrate. In the im-
mediate evaluation, using the universal adhesive in self-
etching mode reduced the m and σ in sound dentin,
while the wet-bonding etch-and-rinse approach resulted in
higher σ. One year of water storage decreased the m for
all groups in CAD, whereas in SD, reductions were noted
only for the universal adhesive applied in the wet-bonding
etch-and-rinse mode and for the control etch-and-rinse
adhesive. Weibull analysis plots for all experimental
groups tested in SD and CAD are depicted in Figs 1 and
2, respectively.

Table 3 Microtensile bond strengths (means ± SD), characteristic strength (σ), Weibull modulus (m) and respec-
tive confidence intervals (95% CI) for all experimental conditions

Storage period 24 h

Etching mode Sound dentin Caries-affected dentin

Substrate

σ m μTBS σ m μTBS

SBU 56.79 (47.69–67.44) 3.14 (1.99–4.23) 50.1(7.4 28.24 (23.56–33.73) 2.87 (1.86–3.81) 23.8(5.0
Wet-bonding E&R

SBU 42.25 (37.09–47.99) 3.20 (2.27–4.09) 47.3(5.5 26.03 (22.39–30.13) 2.89 (2.02–3.71) 23.9(5.3
Dry-bonding E&R

SBU 30.03 (24.10–37.29) 2.49 (1.58–3.36) 28.3(5.5 20.53 (18.31–22.95) 4.13 (2.80–5.39) 20.7(4.2
Self-etching

SB 43.74 (38.80–49.15) 3.63 (2.54–4.67) 43.8(6.4 32.74 (28.02–38.07) 2.61 (1.88–3.31) 26.1(5.5

CSEB 46.90 (41.18–53.24) 3.63 (2.46–4.74) 44.1(6.0 28.70 (26.70–30.78) 5.82 (4.13–7.44) 24.4(4.1

CSEB: Clearfil SE Bond; SB: Adper Single Bond Plus; SBU: Scotchbond Universal adhesive; E&R: etch-and-rinse; (n = 5).

478 The Journal of Adhesive Dentistry

 Lenzi et al

2 2 2 2

1 1 1 1

0 0 0 0

Ln(Ln(1/(1-PF)))
Ln(Ln(1/(1-PF)))

-1 -1 -1 -1

-2 -2 -2
-2

-3 -3
-3 -3

-4 -4
-4 -4

-5 -5
-5 -5 1 2 3 4
1 2 3 4 5
Ln m Ln m
SBU Dry E&R 24 h SBU Dry E&R 24 h SBU Dry E&R 24 h SBU Dry E&R 24 h
SBU Wet E&R 24 h SBU Wet E&R 24 h SBU Wet E&R 24 h SBU Wet E&R 24 h
SBU Self-etch 24 h SBU Self-etch 24 h SBU Self-etch 24 h SBU Self-etch 24 h
SB 24 h SB 24 h SB 24 h SB 24 h
CSEB 24 h CSEB 24 h CSEB 24 h CSEB 24 h
SBU Wet E&R 1 y SBU Wet E&R 1 y SBU Wet E&R 1 y SBU Wet E&R 1 y
SBU Dry E&R 1 y SBU Dry E&R 1 y SBU Dry E&R 1 y SBU Dry E&R 1 y
SBU Self-etch 1 y SBU Self-etch 1 y SBU Self-etch 1 y SBU Self-etch 1 y
SB 1 y SB 1 y SB 1 y SB 1 y
CSEB 1 y CSEB 1 y CSEB 1 y CSEB 1 y

Fig 1 Weibull analysis plots for all experimental groups tested with Fig 2 Weibull analysis plots for all experimental groups tested with
SD. CAD.

The distribution of failure modes is summarized in DISCUSSION

Table 4. In all groups, adhesive/mixed failure prevailed.
Premature failures did not exceed 5% of the total number of Pooled results from a systematic review21 have shown that
tested specimens and were similarly distributed within the the bond strength of universal adhesives to dentin is not
groups. affected by etching strategy. Nonetheless, the results of

1 year

Sound dentin Caries-affected dentin

σ m μTBS σ m μTBS

42.37 (37.65–47.54) 1.93 (1.37–2.47) 35.9(7.0 23.40 (13.66–39.85) 1.08 (0.67–1.48) 18.7(7.1

48.33 (38.89–59.69) 4.00 (2.71–5.22) 36.4(5.9 28.85 (20.79–39.97) 1.91 (1.13–2.65) 18.9(8.2

33.31 (27.81–39.76) 2.87 (1.87–3.82) 24.0(6.7 26.03 (21.19–31.81) 2.29 (1.55–2.99) 18.6(6.5

28.85 (23.31–35.51) 2.12 (1.46–2.75) 24.7(5.7 14.43 (10.70–19.31) 1.51 (1.04–1.96) 13.1(5.1

49.84 (43.95–56.38) 4.37 (2.77–5.89) 39.2(4.0 12.7 (9.91–16.16) 1.82 (1.26–2.37) 11.4(3.4

Vol 18, No 6, 2016 479

Lenzi et al

Table 4 Number and percentage of sticks (%) according to failure mode for all experimental groups

Groups Dentin Storage A/M CR CD Debonded Total

condition period
SBU SD 24 h 28 (66.7) 9 (21.4) 5 (11.9) 0 (0) 42
Wet-bonding E&R 1 year 29 (67.5) 9 (20.9) 4 (9.3) 1 (2.3) 43

CAD 24 h 32 (76.2) 1 (2.4) 9 (21.4) 0 (0) 42

1 year 36 (90.0) 1 (2.5) 1 (2.5) 2 (5.0) 40

SBU SD 24 h 25 (65.8) 8 (21.0) 4 (10.5) 1 (2.7) 38

Dry-bonding E&R 1 year 35 (87.5) 2 (5.0) 3 (7.5) 0 (0) 40

CAD 24 h 24 (66.7) 7 (19.4) 5 (13.9) 0 (0) 36

1 year 31 (88.6) 0 (0) 3 (8.6) 1 (2.8) 35

SBU SD 24 h 31 (73.8) 5 (11.9) 6 (14.3) 0 (0) 42

Self-etching 1 year 33 (82.5) 1 (2.5) 4 (10.0) 2 (5.0) 40

CAD 24 h 25 (71.4) 3 (8.6) 6 (17.1) 1 (2.9) 35

1 year 33 (97.1) 1 (2.9) 0 (0) 0 (0) 34

SB SD 24 h 27 (77.1) 1 (2.9) 7 (20.0) 0 (0) 35

1 year 28 (75.7) 4 (10.8) 5 (13.5) 0 (0) 37

CAD 24 h 30 (71.4) 5 (11.9) 7 (16.7) 0 (0) 42

1 year 36 (90.0) 0 (0) 2 (5.0) 2 (5.0) 40

CSEB SD 24 h 25 (64.1) 6 (15.4) 8 (20.5) 0 (0) 39

1 year 29 (72.5) 2 (5.0) 9 (22.5) 0 (0) 40

CAD 24 h 38 (86.4) 2 (4.5) 1 (2.3) 0 (0) 39

1 year 37 (90.2) 2 (4.9) 0 (0) 2 (4.9) 41

CSEB: Clearfil SE Bond; SB: Adper Single Bond Plus; SBU: Scotchbond Universal adhesive; E&R: etch-and-rinse; SD: sound dentin; CAD: caries-affected dentin;
A/M: adhesive/mixed failure; CD: cohesive failure in dentin; CR: cohesive failure in resin; debonded: prematurely debonded specimens.

studies examining the bond longevity of these adhe-
sives16,18,22 do not agree. While one study demonstrated
that self-etching vs other modes was associated with higher
bond strengths after 1 year of water storage,16 another
found that the performance of universal systems is material
dependent, since adhesives that contained MDP showed
more stable bond strengths after 6 months, irrespective of
the etching approach.18
It should be borne in mind that the studies mentioned
above were performed only in sound dentin of permanent
teeth; hence, different findings could be expected on differ-
ent dental substrates, such as primary teeth and caries-af-
fected dentin. In the current study, the etch-and-rinse or
self-etching strategies of the universal adhesive did not per-
form equally on different dentin substrates.
Resin-bonded interfaces formed in CAD are more com-
plex than in sound dentin, being composed of multiple
zones: resin infiltrated dentin, poorly infiltrated dentin, ex-
posed dentin, and partially demineralized dentin.8 There is
a consensus that CAD results in decreased bond strength,
mainly due to reduced intertubular mineral content.26 Micro-
tensile bond strength data generally exhibit high variability;5
Weibull (m and σ) statistics can describe the bond strength
variations. Lower bonding reliability (lower m) was found in
CAD than in SD, reflecting the influence of histological al-
terations in CAD that create intrinsic flaws at the adhesive
interface.7 However, the association of preliminary phos-
phoric acid and acidic primer application did not jeopardize
the bonding of the universal adhesive to CAD, since no dif-
ference between etch-and-rinse and self-etching strategies
was found in this substrate. On SD, dry-bonding and wet-
bonding etch-and-rinse approaches achieved higher bond
strength than did the self-etching mode. Similarly, the self-
etching approach decreased the m and σ of the universal
adhesive to SD, indicating nonuniform distribution of highly
variable crack lengths.20
Degradation of the resin-dentin bonds was observed
after 1 year of water storage, except when Scotchbond
Universal Adhesive was applied with dry-bonding etch-
and-rinse and self-etching strategies, independent of the
dentin condition. Most studies2,11,19 on the bond stabil-
ity of interfaces created by self-etching adhesive systems
have demonstrated a greater resistance to degradation
than those produced by etch-and-rinse adhesive systems.
The creation of more homogeneous hybrid layers24 and
the protective effect of both resin-coated collagen and
the calcium salts of MDP (10-methacryloxydecyl dihydro-
gen phosphate) formed22 may explain the superior bond
stability. However, in this study, the long-term perfor-
mance of Adper Single Bond Plus and Clearfil SE Bond
was similar. Scotchbond Universal Adhesive contains cer-
tain elements of both these systems, including the poly-
alkenoic acid copolymer (Vitrebond Copolymer) found in
Adper Single Bond Plus and the functional monomer MDP

480 The Journal of Adhesive Dentistry


at a lower concentration than in the self-etching system
Clearfil SE Bond. Although some concern has been ex-
pressed that polyalkenoic acid copolymer may compete
with MDP monomer for calcium-bonding sites in hydroxy-
apatite,25 this study found that the association of these
components promotes more stable resin-dentin bonds,
comparable to those of adhesives considered the gold
standard in each category.
Scotchbond Universal Adhesive is categorized as an ul-
tra-mild self-etching adhesive (pH = 2.7) with a reduced abil-
ity to dissolve the smear layer and demineralize the underly-
ing dentin surfaces.6 Considering the lower mineral content
of primary dentin,1 the use of universal adhesives in self-
etching mode might be sufficient to provide adequate adhe-
sion to this substrate. Nevertheless, Scotchbond Universal
Adhesive applied in self-etching mode to SD resulted in an
approximately 50% lower immediate bond strength in com-
parison with the other groups in this study. Thus, the resin-
dentin bond stability observed when using the universal
adhesive in self-etching mode might be related to the low-
est immediate μTBS and not to a lower decrease in bond
strengths over time. Furthermore, signs of degradation in
restorations of noncarious cervical lesions were found when
using Scotchbond Universal Adhesive in self-etching mode
after 36 months.15 We considered that if the self-etching
approach showed lower bond strengths in the laboratory
study, the universal adhesive might have presented poor
clinical performance when applied in the self-etching vs the
etch-and-rinse mode.
Although the immediate μTBS of the universal adhesive
applied in both dry- and wet-bonding etch-and-rinse modes
were similar, the dry-bonding etch-and-rinse strategy
showed better bond stability over time. The greater amount
of water at the interface when using the universal adhesive
in wet-bonding etch-and-rinse mode could result in inhibition
of resin polymerization and/or monomer dilution,9 compro-
mising the bond longevity.
According to the manufacturer, the combination of Vit-
rebond copolymer, MDP, and silane (“VMS Technology”)
promotes the rehydration of collagen fibrils and hybrid
layer formation even on dry, demineralized dentin. A previ-
ous study9 also found that the dry-bonding etch-and-rinse
protocol was more effective than its wet-bonding counter-
part when a multimode adhesive was tested (G-Bond Plus,
GC; Tokyo, Japan). This result is very interesting, because
the maintenance of adequate moisture is still a clinical
challenge when using etch-and-rinse adhesives. Higher σ
and m were observed for the dry-bonding etch-and-rinse
approach, mainly after water aging. If one adhesive strat-
egy promotes higher m values, it could be considered a
good choice for clinical use, since the increase in m repre-
sents a more uniform distribution of defects on the mater-
ial surface. Thus, Scotchbond Universal Adhesive may be
a suitable alternative to current two-step etch-and-rinse
adhesives.
Vol 18, No 6, 2016
Lenzi et al
CONCLUSION
The dry-bonding etch-and-rinse mode improves the bonding
ability of the universal adhesive tested to sound and artifi-
cially-induced caries-affected primary dentin over time.
ACKNOWLEDGMENTS
We would like to thank CAPES/PNPD for financial support.
REFERENCES
1. Angker L, Nockolds C, Swain M V, Kilpatrick N. Quantitative analysis of
the mineral content of sound and carious primary dentine using BSE im-
aging. Arch Oral Biol 2004;49:99–107.
2. Armstrong SR, Vargas MA, Fang Q, Laffoon JE. Microtensile bond
strength of a total-etch 3-step, total-etch 2-step, self-etch 2-step, and a
self-etch 1-step dentin bonding system through 15-month water storage.
J Adhes Dent 2003;5:47–56.
3. Bengtson CR, Bengtson AL, Bengtson NG, Turbino ML. Do the origins of
primary teeth affect the bond strength of a self-etching adhesive system
to dentin? Braz Oral Res 2010:24:355–360.
4. Bouillaguet S, Gysi P, Wataha JC, Ciucchi B, Cattani M, Godin C,
Meyer JM. Bond strength of composite to dentin using conventional, one-
step, and self-etching adhesive systems. J Dent 2001;29:55–61.
5. Burrow MF, Thomas D, Swain M V, Tyas MJ. Analysis of tensile bond
strengths using Weibull statistics. Biomaterials 2004;25:5031–5035.
6. Cardoso M V, de Almeida Neves A, Mine A, Coutinho E, Van Landuyt K,
De Munck J, Van Meerbeek B. Current aspects on bonding effectiveness
and stability in adhesive dentistry. Aust Dent J 2011;56(suppl 1):31–44.
7. Dickens SH, Cho BH. Interpretation of bond failure through conversion
and residual solvent measurements and Weibull analyses of flexural and
microtensile bond strengths of bonding agents. Dent Mater 2005;21:
354–364.
8. Haj-Ali R, Walker M, Williams K, Wang Y, Spencer P. Histomorphologic
characterization of noncarious and caries-affected dentin/adhesive inter-
faces. J Prosthodont;15:82–88.
9. Hanabusa M, Mine A, Kuboki T, Momoi Y, Van Ende A, Van Meerbeek B,
De Munck J. Bonding effectiveness of a new ‘multi-mode’ adhesive to
enamel and dentine. J Dent 2012;40:475–484.
10. Joves GJ, Inoue G, Nakashima S, Sadr A, Nikaido T, Tagami J. Mineral
density, morphology and bond strength of natural versus artificial caries-
affected dentin. Dent Mater J 2013;32:138–143.
11. Koshiro K, Inoue S, Tanaka T, Koase K, Fujita M, Hashimoto M, Sano H.
In vivo degradation of resin-dentin bonds produced by a self-etch vs. a to-
tal-etch adhesive system. Eur J Oral Sci 2004;112:368–375.
12. Lenzi TL, Braga MM, Raggio DP. Shortening the etching time for etch-and-
rinse adhesives increases the bond stability to simulated caries-affected
primary dentin. J Adhes Dent 2014;16:235–241.
13. Lenzi TL, Calvo AFB, Tedesco TK, Ricci HA, Hebling J, Raggio DP. Effect
of method of caries induction on aged resin-dentin bond of primary teeth.
BMC Oral Health 2015;15:79.
14. Lenzi TL, Raggio DP, Soares FZM, Rocha R de O. Bonding Performance of
a Multimode Adhesive to Artificially-induced Caries-affected Primary Den-
tin. J Adhes Dent 2015;17:125–131.
15. Loguercio AD, de Paula EA, Hass V, Luque-Martinez I, Reis A, Perdigão J.
A new universal simplified adhesive: 36-month randomized double-blind
clinical trial. J Dent 2015;43:1083–1092.
16. Marchesi G, Frassetto A, Mazzoni A, Apolonio F, Diolosà 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.
17. Van Meerbeek B, Yoshihara K, Yoshida Y, Mine A, De Munck J, Van Lan-
duyt KL. State of the art of self-etch adhesives. Dent Mater 2011;27:
17–28.
18. Muñoz MA, Luque-Martinez I, Malaquias P, Hass V, Reis A, Campanha
NH, Loguercio AD. In vitro longevity of bonding properties of universal ad-
hesives to dentin. Oper Dent;40:282–292.
19. Okuda M, Pereira PNR, Nakajima M, Tagami J, Pashley DH. Long-term du-
rability of resin dentin interface: nanoleakage vs. microtensile bond
strength. Oper Dent;27:289–296.
481
Lenzi et al
20. Quinn JB, Quinn GD. A practical and systematic review of Weibull statistics
for reporting strengths of dental materials. Dent Mater 2010;26: 135–147.
21. Rosa WL de O da, Piva E, Silva AF da. Bond strength of universal adhe-
sives: A systematic review and meta-analysis. J Dent 2015;43:765–776.
22. Wagner A, Wendler M, Petschelt A, Belli R, Lohbauer U. Bonding perfor-
mance of universal adhesives in different etching modes. J Dent
2014;42:800–807.
23. Yoshida Y, Van Meerbeek B, Nakayama Y, Yoshioka M, Snauwaert J,
Abe Y, Lambrechts P, Vanherle G, Okazaki M. Adhesion to and decalcifi-
cation of hydroxyapatite by carboxylic acids. J Dent Res 2001;80:
1565–1569.
24. 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.
25. Yoshida Y, Yoshihara K, Nagaoka N, Hayakawa S, Torii Y, Ogawa T,
Osaka A, Meerbeek B Van. Self-assembled nano-layering at the adhesive
interface. J Dent Res 2012;91:376–381.
482
26. Yoshiyama M, Tay FR, Doi J, Nishitani Y, Yamada T, Itou K, Carvalho RM,
Nakajima M, Pashley DH. Bonding of self-etch and total-etch adhesives to
carious dentin. J Dent Res 2002;81:556–560.
27. Zanchi CH, Lund RG, Perrone LR, Ribeiro GA, del Pino FAB, Pinto MB,
Demarco FF. Microtensile bond strength of two-step etch-and-rinse adhe-
sive systems on sound and artificial caries-affected dentin. Am J Dent
2010;23:152–156.
28. Zanchia CH, D’Avila OP, Rodrigues-Junior SA, Burnett LH, Demarco FF,
Pinto MB. Effect of additional acid etching on bond strength and struc-
tural reliability of adhesive systems applied to caries-affected dentin.
J Adhes Dent 2010;12:109–115.
Clinical relevance: The present results support the use
of MDP-containing universal adhesives in dry-bonding
etch-and-rinse mode to promote the long-term success
of minimally invasive restorations in primary teeth.
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