©

Operative Dentistry, 2008, 33-5, 564-570

Effect of Double-application
or the Application of a
Hydrophobic Layer for
Improved Efficacy of One-step
Self-etch Systems in
Enamel and Dentin
M Albuquerque • M Pegoraro
G Mattei • A Reis • AD Loguercio

Clinical Relevance
The double-application and placement of a hydrophobic resin coat can improve the performance
(µTBS) of one-step self-etch systems to tooth substrates, mainly in dentin.

SUMMARY placement of a hydrophobic resin coat) com-

Objectives: To evaluate the use of two alternative
modes of application (double-application and
Maurício Albuquerque, undergraduate student, School of
Dentistry, University of Oeste de Santa Catarina, Joaçaba, SC,
Brazil
Mariana Pegoraro, undergraduate student, School of Dentistry,
University of Oeste de Santa Catarina, Joaçaba, SC, Brazil
Gracielle Mattei, undergraduate student, School of Dentistry,
University of Oeste de Santa Catarina, Joaçaba, SC, Brazil
Alessandra Reis, DDS, PhD, adjunctive professor, School of
Dentistry, Department of Dental Materials and Operative
Dentistry, University of Oeste de Santa Catarina, Joaçaba, SC,
Brazil and Department of Restorative Dentistry, University
Estadual de Ponta Grossa, Ponta Grossa, PR, Brazil
*Alessandro Dourado Loguercio, DDS, MS, PhD, adjunctive pro-
fessor, School of Dentistry, Department of Restorative
Dentistry, University Estadual de Ponta Grossa, Ponta Grossa,
PR, Brazil
*Reprint request: Mestrado em Odontologia, Rua Carlos
Cavalcante, 4748-Bloco M, Sala 64A, Uvaranas Ponta Grossa,
PR, Brazil,84030-900; e-mail: aloguercio@hotmail.com
DOI: 10.2341/07-145
pared with the manufacturers’ directions on the
microtensile bond strength (µTBS) of one-step,
self-etch systems to enamel and dentin.
Materials and Methods: Resin composite
buildups were bonded to the buccal and lingual
ground enamel surfaces and occlusal dentin of
third molars using the following adhesives: Xeno
III (XE), GBond (GB), Adper Prompt L-Pop (AD)
and Clearfil SE Bond (CSE) as the control. The
adhesive systems were applied: 1) following the
manufacturer’s directions (MD), 2) with double-
application (DA) or with 3) additional placement
of a hydrophobic resin layer (HR) after following
the manufacturer’s directions. After storage in
water (24 hours/37°C), the bonded specimens
were sectioned into sticks (0.8 mm2) that were
tested until failure at a crosshead speed of 0.5
mm/minute. Data from each substrate were sub-
jected to two-way ANOVA and Tukey’s test
(α=0.05).
Results: The interaction Adhesive vs
Application mode was statistically significant
Albuquerque & Others: One-step Self-etch Systems: Changing the Application Mode
(p<0.05) for both substrates. In dentin, XE and GB
achieved high µTBS in the HR group (p<0.05).
For AD, the highest µTBS were observed in the
DA group (p<0.05). For enamel, similar µTBS was
observed for XE and GB among the three modes
of application, while the highest µTBS of AD was
observed in the HR group.
Conclusion: The effects of using the double-
application and placement of a hydrophobic
resin coat on microtensile dentin-bond strength
values seem to be effective; however, these tech-
niques in enamel were adhesive-dependent.
INTRODUCTION
Today, bonding to tooth hard tissue can be accom-
plished by using one of two adhesion strategies: the
etch-and-rinse or the self-etch approach. Contrary to
the etch-and-rinse approach, the conditioning step in
self-etch systems is not separated from the priming
step and, therefore, demineralization and infiltration
occurs simultaneously, at least from a theoretical view-
point.1 Another difference from the etch-and-rinse
approach is that the tooth is no longer rinsed, which not
only lessens clinical application time, but also signifi-
cantly reduces technique-sensitivity. Self-etch systems
are also more user-friendly than the etch-and-rinse
approach, as the separate etching step and the conse-
quential management of dentin moisture was com-
pletely eliminated.1
Initially, self-etch adhesives were introduced for use
in a two-step procedure. After application of an acidic
primer, a relatively hydrophobic bonding resin was to
be applied on top of the primed surface. However,
recently, the trend related to developing new
dentin/enamel adhesives has focused on simplification
of the clinical steps involved in the bonding protocol.
One-step self-etch systems (also known as all-in-one)
were introduced. The manufacturers of these products
attempted to incorporate all of the components of an
adhesive system (etchant, primer and bonding resin)
into a single solution, resulting in a reduced-step, user-
friendly adhesive. As these materials have become pop-
ular among clinicians,2 they are being introduced at a
very fast rate, without comprehensive testing to sub-
stantiate their performance.
Different research centers have shown that some one-
step self-etch adhesives exhibit relatively low bond
strength values to both enamel and dentin, when com-
pared to two-step self-etch or etch-and-rinse systems.3-5
This inferior performance has been attributed to cer-
tain factors. First, these products create very thin coat-
ings,6-8 which may be oxygen inhibited, resulting in a
poorly polymerized adhesive layer.9 Second, they are
highly prone to phase separation10 as the solvent evap-
orates from the solution and, finally, they behave as
565
permeable membranes after polymerization.11 The lat-
ter is due to the presence of water-attracting
hydrophilic domains12 and interconnecting water-filled
channels (water-trees) within the polymerized adhe-
sives, permitting water to move from the underlying
dentin through the adhesive.13
Some authors have indicated that treating one-step
self-etch systems as a primer and covering them with a
less hydrophilic resin coating (converting them into
two-step materials) can be an option for resolving their
drawbacks.8,14-15 Other authors, however, have suggest-
ed placing multiple layers6-8 in a clinical attempt to
improve their clinical efficacy. Despite these positive
findings, the performance of the above mentioned alter-
native techniques seem to be dependent on the brand of
adhesive tested.15-17 In addition, hardly any attention
has been given to the enamel substrate, as most of the
previously cited studies were conducted in dentin.
Concerns regarding the bonding efficacy of one-step
self-etch systems to enamel have recently been raised.
It was demonstrated that employing simplified self-
etch adhesives in enamel can result in osmotic blister-
ing and, consequently, bond failure when they are not
covered by a hydrophobic resin layer or a resin compos-
ite.18
Thus, this study evaluated two alternative modes of
application for one-step self-etch adhesive systems
(multiple coats and placement of a hydrophobic resin
coat) and compared them with the manufacturers’
directions on ground enamel and dentin.
METHODS AND MATERIALS
Three one-step self-etch adhesive systems were tested:
Adper Prompt L-Pop (AD, 3M ESPE, St Paul, MN,
USA), Xeno III (XE, Dentsply De Trey, Konstanz,
Germany) and G-Bond (GB, GC, Tokyo, Japan). Clearfil
SE Bond (CSE, Kuraray, Osaka, Japan), a two-step
self-etch adhesive system, was used as the control. The
composition, application mode and batch number are
described in Table 1.
Ninety extracted, caries-free human third molars
were used. The teeth were collected after obtaining the
patients’ informed consent under a protocol approved
by the University of Oeste of Santa Catarina
Institutional Review Board. The teeth were disinfected
in 1% thymol stored in distilled water and used within
six months of extraction. For dentin, 60 teeth were
used. A flat dentin surface was exposed after wet grind-
ing the occlusal enamel on #180 grit SiC paper. The
exposed dentin surfaces were further polished on wet
#600-grit silicon-carbide paper for 60 seconds to stan-
dardize the smear layer.
For enamel, 30 teeth were employed. They were sec-
tioned in a mesio-to-distal direction in order to obtain
buccal and lingual tooth halves. These surfaces were
566 Operative Dentistry

Table 1: Adhesive Systems: Composition, Batch Number and Application Mode of Different Groups
Adhesive Systems
(manufacturer) Composition (batch #)
Clearfil SE Bond Primer—water, MDP, HEMA,
(Kuraray) camphoroquinone, hydrophilic
dimethacrylate (00176A);
Adhesive—MDP, Bis-GMA,
HEMA, camphoroquinone,
hydrophobic dimethacrylate,
N,N-diethanol p-toluidine bond,
colloidal silica (001185A)
Adper Prompt Liquid A—water, MDP, HEMA,
L-Pop camphoroquinone and hydrophilic
(3M ESPE) dimethacrylate (225666);
Liquid B—water, HEMA,
polyalkenoic acid, stabilizers
(250246)
Xeno III (Dentsply) Liquid A: HEMA, ethanol, water,
aerosil, stabilizers (0601002833)
Liquid B: Pyro-EMA, PEM-F,
UDMA, canforquinone, stabilizers,
ethyl-4-dimethylaminobenzoate
(cointiator) (0601002832)
G Bond (GC Corp) 4-MET, UDMA, phosphate
monomer, DMA component,
fumed silica filler, acetone, water
and photoinitiator (0606231)
MDP: methacryloyloxydodecylpyridinium; HEMA: 2-hydroxyethyl methacrylate; Bis-GMA: bisphenol A diglycidyl methacrylate; 4-MET: 4-methacryloyloxyethyl trimellitic acid; Pyro-EMA: tetram-
ethacryloyloxyethyl pyrophosphate; PEM-F: pentamethacryloyloxyethylcyclohexaphosphazene monofluoride; UDMA: urethane dimethacrylate; DMA: dimethacrylate
Application Mode
Manufacturers’ Directions (MD) Double- Hydrophobic
Application (DA) Resin Layer (HR)
1. Apply two coats of the primer under 1. Steps 1 through 4 from MD; 1. Steps 1 through 5
pressure (20 seconds); 2. Repeat steps 1 through 4; from MD;
2. Air stream (10 seconds at 20 cm) after 3. Step 5 2. Repeat steps 4
application of each coat; through 5.
3. Apply one coat of the adhesive (15
seconds);
4. Air stream to make the bond film uniform
(3 seconds at 20 cm);
5. Light-activation (10 seconds—600 mW/cm2).
1. Mix liquids A and B for 5 seconds; 1. Steps 1 through 5 from MD; 1. Steps 1 through 6 from
2. Apply one coat of the adhesive under 2. Repeat steps 2 through 5; MD;
pressure (15 seconds); 3. Step 6. 2. Apply one coat of
3. Gentle air stream (10 seconds at 20 cm); adhesive from CSE;
4. Apply a second coat of the adhesive under 3. Air stream to make
pressure (15 seconds); the bond film uniform
5. Gentle air stream (10 seconds at 20 cm); (3 seconds at 20 cm);
6. Light-activation (10 seconds—600 mW/cm2). 4. Light-activation (10
seconds—600 mW/cm2).
1. Mix liquids A and B for 5 seconds 1. Steps 1 through 3 from MD; 1. Steps 1 through 4
2. Apply one thick coat of the adhesive under 2. Repeat steps 2 and 3; from MD;
pressure (30 seconds); 3. Step 4. 2. Apply one coat of
3. Gentle air stream (10 seconds at 20 cm); adhesive from CSE;
4. Light-activation (10 seconds—600 mW/cm2). 3. Air stream to make
the bond film uniform
(3 seconds at 20 cm);
4. Light-activation (10
seconds—600 mW/cm2).
1. Apply one coat of adhesive, scrub for 5 1. Steps 1 through 3 from MD; 1. Steps 1 through 4 from
seconds; 2. Repeat steps 1 through 3; MD;
2. The adhesive was left undisturbed 3. Step 4. 2. Apply one coat of
for 5-10 seconds; adhesive from CSE;
3. Air dry under maximum pressure for 5 3. Air stream to make
seconds; the bond film uniform
4. Light-curing for 10 seconds at (3 seconds at 20 cm);
600 mW/cm2. 4. Light-activation (10
seconds—600 mW/cm2.

cleaned with slurry of pumice and water and examined
under a 40x stereomicroscope (HMV-2, Shimadzu,
Tokyo, Japan) to ensure that the teeth were free of sur-
face cracks, decalcification or any sign of previous
grinding. Upon completion of the examination, the
enamel was demarcated to outline the flattest area for
bonding. The mid-coronal third of the buccal and lin-
gual surfaces were usually outside the bonding area
due to their inclination. The demarcated enamel sur-
faces were then flattened with a fine-grit diamond bur
(#2135F, KG Sorensen, Barueri, São Paulo, Brazil)
attached to a high-speed handpiece under water irriga-
tion to remove the superficial 0.5 mm enamel layer. The
abraded surfaces were then polished with wet 600-grit
SiC paper to produce a standard smear layer.
For each substrate, the adhesives listed in Table 1
were applied to enamel according to three different
modes. In the MD group, the adhesive systems were
applied according to the manufacturers’ directions
(Table 1). In Group DA, each adhesive system was
applied following the manufacturer’s directions; howev-
er, the number of recommended coats was duplicated
(double-application). In the HR group, each adhesive
system was applied according to each manufacturer’s
directions, however, each tooth received an additional
coat of a hydrophobic resin layer (Bond bottle, Clearfil
SE Bond).
The adhesives were light cured for the recommended
time (Table 1) using a VIP light unit set at 600 mW/cm2
(BISCO, Schaumburg, IL, USA). Resin composite
build-ups (Z250, 3M ESPE, St Paul, MN, USA) were
constructed on the bonded surfaces in three increments
of 1 mm each, which were individually light cured for
30 seconds with the same light intensity. All the bond-
ing procedures were carried out by a single operator at
a room temperature of 24°C and constant relative
Albuquerque & Others: One-step Self-etch Systems: Changing the Application Mode 567

humidity. Five teeth (dentin) and five hemi-teeth The data from each substrate were subjected to two-
(enamel) were used for each combination of the factors way ANOVA (Adhesive vs Application Mode) and
Adhesive vs Application mode. Tukey’s test for pairwise comparisons at a pre-signifi-
After the restored teeth were stored in distilled water cant level of α=0.05. For enamel, an additional random
at 37°C for 24 hours, they were longitudinally sectioned factor was added to the statistical model as correction
in both the “x” and “y” directions across the bonded for the two half samples gathered from the same tooth.19
interface using a diamond saw in a Labcut 1010 RESULTS
machine (Extec Corp, Enfield, CT, USA) to obtain
sticks, each with a cross-sectional area approximately Dentin
0.8 mm2. The number of premature debonded sticks (D) The mean cross-sectional area ranged from 0.80 to 0.92
per tooth during specimen preparation was recorded. mm2 and no difference among the groups was detected
The cross-sectional area of each stick was measured (p>0.05). The mean and standard deviations of the
with the digital caliper (Absolute Digimatic, Mitutoyo, resin-dentin µTBS means (MPa) are depicted in Table
Tokyo, Japan) to the nearest 0.01 mm for calculation of 2, as well as the number of tested vs premature debond-
the actual microtensile bond strength values (µTBS). ed sticks. The interaction of the Adhesive vs Application
Each bonded stick was attached to a modified device Mode was statistically significant (p=0.0001). As seen in
for microtensile testing with cyanoacrylate resin (Zapit, Table 2, CSE, AD and XE applied according to the man-
Dental Ventures of North America, Corona, CA, USA) ufacturers’ directions showed resin-dentin µTBS means
and subjected to a tensile force in a universal testing inferior to those obtained in the DA (double-application)
machine (EMIC, São José dos Pinhais, PR, Brazil) at a and HB (hydrophobic bonding layer) groups. For XE
crosshead speed of 0.5 mm/minute. The failure modes and GB, the highest resin-dentin µTBS were obtained
were evaluated at 400x (HMV-2, Shimadzu, Tokyo, under the HB group (p<0.05), while for AD, the highest
Japan) and classified as cohesive ([C] failure exclusive µTBS were observed under the DA group (p<0.05). The
within dentin or resin composite), adhesive ([A], failure CSE adhesive, used as the control, showed similar
at the resin/dentin interface) or adhesive/mixed ([A/M], resin-dentin µTBS under all experimental conditions
failure at the resin/dentin interface, which included (p>0.05).
cohesive failure of the neighboring substrates). Enamel
The resin-dentin and resin-enamel bond strength of The mean cross-sectional area ranged from 0.73 to 0.90
all sticks with adhesive or mixed fracture mode from mm2 and no difference among the treatment groups
the same tooth (dentin) or hemi-tooth (enamel) were was detected (p>0.05). The mean and standard devia-
averaged for statistical purposes. The premature tions of the resin-enamel µTBS means (MPa) are
debonded specimens were also included in the mean. depicted in Table 3, as well as the number of tested vs
The value attributed to these specimens was half of the premature debonded sticks. The interaction Adhesive
minimum bond strength value measured in the current vs Application mode was statistically significant
study for each substrate. (p=0.03). As seen in Table 3, XE and GB applied accord-
ing to the manufac-
Table 2: Microtensile Resin-dentin Bond Strength Values (MPa): Means and Standard Deviations
turers’ directions
(number tested/premature debonded sticks) showed resin-
enamel µTBS
Adhesive Manufacturer’s Directions Double Application Hydrophobic Resin Layer means similar to or
CSE 18.0 ± 4.7 (30/05) f 25.2 ± 1.6 (29/04) e,f 24.5 ± 4.6 (35/04) e,f higher than the DA
AD 24.3 ± 3.1 (28/09) e,f 45.3 ± 6.4 (28/01) a,b 29.5 ± 4.9 (36/14) d,e or HB groups
XE 30.0 ± 1.2 (26/07) d,e 33.8 ± 3.4 (24/07) c,d 49.8 ± 3.7 (29/02) a (p>0.05); however,
GB 37.1 ± 2.4 (38/06) b,c,d 20.6 ± 3.9 (31/04) f 44.5 ± 3.7 (27/03) a,b GB showed a ten-
*Groups identified with the same letters are not statistically different (p<0.05). dency towards
superior perform-
ance under the HB
Table 3: Microtensile Resin-enamel Bond Strength Values (MPa): Means and Standard Deviations group. For AD, the
(number tested/premature debonded sticks) higher µTBS val-
Adhesive Manufacturer’s Directions Double Application Hydrophobic Resin Layer ues were found in
CSE 33.1 ± 7.9 (18/03) a 22.7 ± 5.0 (20/04) b 25.8 ± 7.1 (17/04) a,b the HB group
AD 13.5 ± 5.4 (14/02) c 17.9 ± 4.7 (24/05) b,c 23.1 ± 5.8 (21/04) b
(p<0.05). The CSE
system, used as the
XE 20.1 ± 4.3 (15/06) b 21.2 ± 7.4 (18/07) b 15.3 ± 4.4 (17/05) b,c
control, showed
GB 25.3 ± 5.6 (16/03) a,b 28.9 ± 6.8 (22/04) a,b 32.0 ± 8.2 (18/04) a
*Groups identified with the same letters are not statistically different (p<0.05).
568
lower resin-enamel µTBS values in the DA group
(p<0.05).
DISCUSSION
The double application of Adper Prompt L-Pop
enhanced the performance of this material to dentin.
This finding was already demonstrated by previous lit-
erature findings, which reported that the application
of only one coat of Adper Prompt L-Pop is not enough
to adequately create a sufficiently thick hybrid and
adhesive layer that will couple to subsequently applied
resin composite.6-8 The increased resin-dentin µTBS
under double application is due to several mechanisms
operating simultaneously. As the solvent is evaporated
between each coat, the concentration of co-monomers
that exist after each coating increases,8 thereby
improving the quality of the hybrid layer20 and the
ratio of the polymerized vs unpolymerized adhesive
layer due to oxygen inhibition.21 According to
Hashimoto and others,20 the improved bonding per-
formance when multiple coats are applied but not
cured cannot be attributed to the increase in adhesive
thickness but to the improved quality of the adhesive
layer. Only when each coat is light-cured, is the thick-
ness of the adhesive layer increased.8
On the other hand, no improvement in resin-dentin
µTBS values was observed for Xeno III and G-Bond
with double application. One important difference
between XE and GB in relation to AD is their filler con-
tent. Filled adhesives, such as XE and GB, produce a
thicker adhesive layer with only one coat,16,22 resulting
in this layer being less susceptible to oxygen inhibi-
tion.21 That is why the manufacturers of unfilled adhe-
sives often recommend the application of at least two
coats of adhesives. This ensures that the etched dentin
will be adequately covered, reducing the deleterious
effects of oxygen inhibition, such as defective bond for-
mation both to self-etch6-8 and etch-and-rinse sys-
tems.23
For G-Bond, the resin-dentin µTBS was statistically
decreased after double application. The rationale
behind this finding was not clearly identified by the
authors of the current investigation. The most plausi-
ble explanation is likely to rely on the solvent differ-
ences between G-Bond and Xeno III. While Xeno III is
composed of a mixture of water and ethanol, G-Bond
contains water and acetone as solvents. As the evapo-
ration of acetone is much faster than water, after ace-
tone evaporation, the water content and monomer con-
centration is increased proportionally, reducing fur-
ther water evaporation. This situation can be even
worse under double-application, permitting water-
accumulation in the adhesive layer. The water mole-
cules compete with the adhesive monomers for binding
sites on collagen, and this might have caused reduc-
tions in resin-dentin µTBS.24-25
Operative Dentistry
Contrary to G-Bond, Xeno III contains a mixture of
water-ethanol as the solvent. This mixture at a specif-
ic ratio (95.6% ethanol and 4.4% water) creates
azeotrope, which is a mixture of two or more miscible
liquids that retain the same composition in vapor as in
liquid state when distilled or partially evaporated
under certain pressure.26 This implies the formation of
hydrogen bonds between water and ethanol molecules,
resulting in better evaporation of these water-ethanol
aggregates than pure water. In addition, the formation
of hydrogen bonds is much lower with ketones (ace-
tone) than with alcohol.27
The additional application of a hydrophobic solvent-
free resin layer improved the performance of Xeno III
and G-Bond in dentin. When one-step self-etch sys-
tems were applied according to a two-step protocol, the
additional application of the hydrophobic bonding
layer must have increased concentration of the
hydrophobic monomers, reducing the relative concen-
tration of solvents and hydrophilic monomers within
the adhesive interface, which explains increased
µTBS. This finding was already demonstrated by pre-
vious literature findings.8,14-15 The application of a
hydrophobic coat also seems to limit the diffusion of
water through the hybrid layer to the interface
between the adhesive and resin composite, otherwise,
this diffusion might have occurred rapidly.11,28 The
additional layer of hydrophobic adhesive increased the
thickness of the adhesive layer, which is known to
reduce polymerization stresses29 and improve stress
distribution during testing.
In regard to enamel substrate, a different scenario
was detected. In fact, no significant improvement was
shown with double-application. One could expect that
this technique would improve the quality of the adhe-
sive layer, leading to better bonding to both sub-
strates.8,21,30 Obviously, one cannot rule out the fact that
the improvement of the adhesive layer properties
might have occurred; however, it seems that this fact
was of less importance for resin-enamel strength.
These results are similar to those reported by Perdigão
and others.31 They showed that the double-application
of Adper Prompt L-Pop did not improve bond strength
to ground enamel.
In regard to the additional application of a hydropho-
bic solvent-free resin layer, no significant improvement
was observed, except for the AD system. Previous lit-
erature findings have demonstrated that low-pH self-
etch systems, such as AD, do not present good per-
formance on tooth substrates3-5 despite their creating a
deeper etching pattern than moderate and less acidic
self-etch systems.32 These findings can be attributed to
the low cohesive strength of the adhesive layer formed
by the AD system. It was already demonstrated that
the cohesive strength of the adhesive layer may be
more important than the etching potential of an enam-
Albuquerque & Others: One-step Self-etch Systems: Changing the Application Mode
el adhesive.33-34 By increasing the mechanical proper-
ties of the adhesive layer through the inclusion of
hydrophobic monomers, the application of an extra
coat of a hydrophobic layer improved the resin-enamel
bond strength values of the AD system.
CONCLUSIONS
The results of the current investigation showed that
the alternative modes of application can lead to differ-
ent results, depending on the material and substrate
that prevents researchers from suggesting the use of
these alternative modes of application for all one-step
systems.
Acknowledgement
This study was partially supported by CNPq grant 473101/2006-
8 and 305870/2004-1.
(Received 15 October 2007)
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