d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1542–1548

available at www.sciencedirect.com

journal homepage: www.intl.elsevierhealth.com/journals/dema

Dentin regional bond strength of self-etch and

total-etch adhesive systems

Jatyr P. Proença a , Mário Polido b , Estrella Osorio a , Maria Carolina G. Erhardt a ,

Fátima S. Aguilera a , Franklin Garcı́a-Godoy c , Raquel Osorio a , Manuel Toledano a,∗
a Department of Dental Materials, School of Dentistry, University of Granada, Campus Cartuja s\n, 18071 Granada, Spain
b Department of Dental Materials, Instituto Superior de Ciências da Saúde-Sul, Monte da Caparica, Portugal
c Clinical Research Center, College of Dental Medicine, Nova Southeastern University, Fort Lauderdale, FL, USA

a r t i c l e i n f o a b s t r a c t

Article history: Objectives. To evaluate the microtensile bond strength (MTBS) of self-etch (with or without
Received 21 March 2006 H3 PO4 -etching) and total-etch bonding systems bonded to different regions of dentin.
Received in revised form Methods. Long flat dentin cavity preparations extending from top-crown to root-apex within
11 January 2007 the same tooth were performed and bonded: using two-step (Clearfil SE Bond/SEB, Resul-
Accepted 6 February 2007 cin Aqua Prime/RES) and one-step (Etch & Prime 3.0/EP, One-Up Bond F/OUB, Prompt
L-Pop/PLP, Solist/SOL and Futurabond/FUT) self-etch adhesives; these same adhesives were
also applied following H3 PO4 -etching of dentin and finally two more groups were bonded
Keywords: with total-etch adhesives (Single Bond/SB and Prime & Bond NT/PBNT). Build-ups of resin
Self-etch composite were constructed incrementally to ensure sufficient bulk for the MTBS test and
Total-etch the different regions of dentin were identified by painting with different colours on the top
Bond strength of the resin composite. Specimens were sliced into beams and tested in tension. ANOVA
Dentin regions and multiple comparisons tests were used (p < 0.05).
Adhesion Results. Regardless of the tested dentin region, SEB attained the highest MTBS to smear layer-
covered surfaces (i.e., coronal dentin: 42.7 MPa), while H3 PO4 -etching of dentin hampered
bonds (i.e., coronal dentin: 27.7 MPa). When bonding with PBNT, SB, RES, EP, PLP, SOL and
FUT, MTBS was similar for different dentin regions. H3 PO4 -etching of dentin did not alter
the attained MTBS.
Significance. SEB yielded the highest MTBS to all regions of dentin. When bonding to parallel-
cut dentin, previous H3 PO4 -etching of dentin did not increase MTBS and differences in bond
strength among dentin regions were absent.
© 2007 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

1. Introduction Efficacy of current adhesive systems is regularly evaluated by

their ability to bond to coronal dentin, nevertheless, develop-
Bonding to dentin has been referred to be a less reliable ments in periodontology significantly increased the demand
and predictable technique when compared to enamel bond- for restoration of root dentin defects [4]. In these clini-
ing [1,2]. Dentin is a hydrated complex composite material cally relevant substrates, the structural anisotropy found due
composed of a collagen-based organic matrix with hydrox- to physiological and pathological alterations imply that the
yapatite reinforcement, varying with anatomical location [3]. nature of the dentin substrate presented for bonding also vary,

∗
Corresponding author. Tel.: +34 958243788; fax: +34 958240908.
E-mail address: toledano@ugr.es (M. Toledano).
0109-5641/$ – see front matter © 2007 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.dental.2007.02.001
 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1542–1548 1543

and discrepancies in bond strengths might be encountered tion were selected. Outer enamel and dentin were removed
[3]. from both the mesial and distal tooth surfaces by means of
A number of new adhesive systems have been developed in 180-grit silicon carbide papers. A long flat cut was performed
an attempt to obtain a reliable bonding to dentin. Two differ- into middle dentin extending from the occlusal-crown to the
ent approaches are the most frequently used. The total-etch apex of the root within the same tooth [4], exposing three
technique relies on the removal of the smear layer and expo- different dentin regions: cuspal or coronal, cervical (near the
sure of the collagen matrix by acid etching [5], followed by the dentin–enamel junction) and root region, that was approxi-
application of a self-priming agent that combines the primer mately 3 mm below the dentin–enamel junction.
and the adhesive resin into one solution [6]. Further incom- Composition, manufacturers, and application protocol of
plete expansion of collagen may impair resin infiltration and the tested adhesives are displayed in Table 1. The total-etch
compromise bonding with these systems [7,8]. The second bonding agents were applied according to manufacturers’
approach is the use of self-etching primers, in which the acid directions. The self-etch systems were applied following man-
and the primer are combined in one solution to form an acidic ufacturers’ instructions or after previous 36% H3 PO4 -etching
monomer [9] and a final bonding step is later applied. Current (Dentsply/DeTrey, Konstanz, Germany—lot # 041210) of dentin.
trends in adhesive technology are directed towards the one- Dentin was etched for 15 s and rinsed for 10 s. The pH of the
step self-etch systems, which have the bonding mechanism bonding agents was assessed using pH indicator strips (Merck
based upon the simultaneous etching, priming and bonding KgaA, Darmstadt, Germany).
to the smear-covered dental tissue using one single solution Resin build-ups, each 6 mm in height, were constructed
[10,11]. Reducing the steps of the adhesive procedure shortens incrementally (2 mm) with Tetric Ceram (Ivoclar Vivadent,
the application time, and leads to a lower technique sensitivity Schäan, Liechtenstein—lot # H09718) light-cured hybrid com-
[12]. When using all these self-etching systems less discrep- posite resin. Each layer of the composite was separately
ancy is expected between the depth of demineralisation and light-activated for 40 s with a Translux EC halogen light-curing
depth of resin infiltration [9,13]. However, the benefit of sav- unit (Kerr Demetron, Danbury, CT, USA). Light intensity output
ing time may be achieved at the expense of compromising was monitored with a Curing Radiometer (Danville Engineer-
the quality of resin–dentin bonds [2,14,15], as these adhesives ing Co., Danville, CA, USA) to be at least 600 mW/cm2 . The
contain highly hydrophilic and acid monomers that make different regions of dentin were identified (coronal, cervical
hybrid layers more permeable and sensitive to water sorption and root thirds) and painted with different colours on the top
from the underlying dentin [16,17]. The self-etching adhesives of the composite.
vary in their acidity by virtue of the composition and con- After storage in distilled water at 37 ◦ C for 24 h, teeth were
centration of polymerizable acids and acidic resin monomers longitudinally sectioned in a buccal-lingual direction from its
[18,19]. central part, yielding two halves, each one containing the
Previous studies suggested that bonding of self-etching resin-bonded dentin surfaces. Specimens were then vertically
adhesive systems to cervical and root dentin may be improved sectioned into serial slabs, and further into beams with cross-
by modifications to protocols that are normally employed to sectional areas of 1 mm2 , following the method described by
coronal dentin [20,21,22], which include the removal of surface Shono et al. [21]. Six molars were performed per group, and
hypermineralized layer by pre-treatment with stronger acids each molar gathered 3–4 beams from each dentin region, hav-
the mineralized components of the smear layer that are effi- ing been obtained 20–24 beams per group and dentin region.
cient buffers, making the pH of acidic monomers too high to All beams were attached to a modified Bencor Multi-T
demineralize the underlying dentin [23]. Although self-etching testing apparatus (Instron Inc., Canton, MA, USA) with a
adhesives etch and prime the dentin surface simultaneously, cyanoacrylate adhesive (Zapit/Dental Ventures of America
previous etching should be considered as it produces a wet- Inc., Corona, CA, USA) and stressed to failure in tension using
table surface due to the removal of the smear layer [1,2], a universal testing machine (Instron Inc., Canton, MA, USA) at
helping for the infiltration of the resin monomers through the a crosshead speed of 0.5 mm/min. The fractured beams were
demineralized interfibrillar spaces [18,20]. carefully removed from the apparatus and the cross-sectional
The aim of this study was to determine the microtensile area at the site of failure was measured to the nearest 0.01 mm
bond strength of two- and one-step self-etch bonding agents with a pair of digital calipers (Sylvae Ultra-Call/Fowler Inc.,
– previously treated or not with 36% phosphoric acid – com- Newton, MA, USA). Fractured specimens were examined with
pared to total-etch systems, when bonded to different dentin a stereomicroscope (Olympus/DeTrey, Konstanz, Germany) at
regions (coronal, cervical and root dentin). The null hypothe- 40× magnification to determine the mode of failure (adhesive,
sis to be tested was that there was no significant difference in cohesive or mixed).
bond strengths of the different adhesive approaches (with or Bond strength data were analyzed with ANOVA and Stu-
without prior application of phosphoric acid when using self- dent Newman Keuls multiple comparisons tests. Statistical
etching systems) and systems (self-etching versus total-etch significance was set in advance at the 0.05 probability level.
adhesives) when applied to coronal, cervical or root dentin.

3. Results
2. Materials and methods
The pH values of the primers of each adhesive system are
Ninety-six caries-free extracted human third molars stored at shown in Table 1. Mean MTBS values obtained in each group
4 ◦ C in 0.5% chloramine T for up to 1 month following extrac- are described in Table 2. Mean bond strength was affected by
 1544
Table 1 – Information about tested adhesive systems
Adhesive Components Principle ingredients Mode/steps of application

Clearfil SE Bond (SEB) – Kuraray Co. Ltd., Osaka, Japan – lot # 41158 (pH 1.9)
Primer 10-MDP; HEMA; hydrophilic dimethacrylate; dl-camphorquinone; Apply primer for 20 . Mild air stream. Apply bond.
N,N-diethanol-p-touidine; water Gentle air stream. Light cure for 10
Two-step self-etch
Bond 10-MDP; bis-GMA; HEMA; hydrophobic dimethacrylate;
di-camphorquinone; N,N-diethanol-p-toluidine; silanated colloidal
silica.
Resulcin AquaPrime + monobond (RES) – Merz Dental, Lütjenburg, Germany – lot # 99490191 (pH 1)
AquaPrime 2-Methacryloyloxyethyl-dihydrogen-phosphate Mix AquaPrime with water (1:1). Scrub into dentin
Monobond Bis-GMA, TEGDMA, polymethacryl-oligomaleic acid surface for 30 . Gently air dry. Apply monobond. Air
blow gently. Light cure for 20
One-up bond F (OUB) – Tokuyama Europe GmbH, Dusseldorf, Germany – lot # 513 (pH 1.3)

d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1542–1548
Agent A Phosphoric monomer, MAC-10, multifunctional methacrylic Mix bonding A and B (1:1). Apply mixed material for
monomer, co-initiator 90 . Gently air stream. Light cure for 20
Agent B Monofunctional monomers, water, fluoroaluminosilicate microfiller,
dye-sensitizer, borate derivative catalyst
Etch & prime 3.0 (EP) – Degussa AG, Hanau, Germany – lot # 019920 (pH 0.76)
One-step self-etch Universal HEMA, water, ethanol, stabilizer Mix Universal and Catalyst. Apply for 30 . Air blow
Catalyst HEMA, initiators, stabilizers, gently. Light cure for 10 . Repeat previously
tetra-methacryloyloxyethylpyrophosphate mentioned steps
Prompt L-Pop (PLP) – 3M ESPE, St. Paul, MN, USA – lot # 41926 (pH 0.7)
Red blister Bis-GMA, methacrylated phosphoric esters, CQ, stabilizers Pack activating. Scrub first coat 15 . Gently air dry.
Yellow blister Water, zinc-fluoride complex, stabilizers Light-cure 10 . Second coat application (scrubbing)
Solist (SOL) – DMG GmbH, Hamburg, Germany – lot # 99450003 (pH 1.8) 15 . Gently air dry. Light-cure 10
HEMA, TEGDMA, acetone, catalyst/stabilizer, elastomers Apply adhesive for 30 . Air blow gently. Light cure for 10 . Apply a
second coat for 5 . Air blow gently. Light cure for 10
Futurabond (FUT) – Voco GmbH, Cuxhaven, Germany – lot # 01148E1 (pH 1)
Bis-GMA, diurethanedimethacrylate, hydroxyethylmethacrylate, BHT, Apply adhesive (scrubbing) for 30 . Air blow gently. Light cure for 20 .
acetone, organic acids Apply adhesive. Air blow gently. Leave second coat uncured

Total-etch Prime & Bond NT (PBNT) – Dentsply/DeTrey, Konstanz, Germany – lot # 0403000422 (pH 2.4)
PENTA, UDMA resin, Resin R5-62-1, T-resin, D-resin, nanofiller, H3 PO4 etch for 15 . Rinse with water spray for 15 . Leave a moist
initiators, stabilizer, cetylamine hydrofluoride, acetone surface with a soft blow of air. Saturate the surface with ample
amounts of the adhesive, reapply if necessary. Leave the surface
undisturbed for 20 . Air blow gently for 5 . Light cure for 10
Single Bond (SB) – 3M ESPE, St. Paul, MN, USA – lot # 040314 (pH 4.3)
HEMA, water, ethanol, amines, bis-GMA, methacrylate-functional, H3 PO4 conditioning for 15 . Rinse with water spray for 10 , leaving
copolymer of polyacrylic and polyitaconic acids, dimethacrlates tooth moist. Apply two consecutive coats of the adhesive with a fully
saturated brush tip. Dry gently 5 . Light cure 10

10-MDP: 10-methacryloxydecyl dihydrogen phosphate; HEMA: 2-hydroxyethyl methacrylate; bis-GMA: bis-phenol A diglycidylmethacrylate; TEGDMA: triethylene glycol-dimethacrylate; MAC-10:
methacryloyloxyalkyl acid phosphate; CQ: camphoroquinone; BHT: butylated hydroxy toluene; PENTA: penta-acrylate ester; UDMA: urethane dimethacrylate.
 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1542–1548 1545

the adhesive system (F = 8.648; p < 0.001), dentin pre-treatment

(F = 11.968; p < 0.001), and dentin region (F = 6.715; p < 0.001).

20.5 (7.7) Ab
22.8 (6.3) Ab
18.0 (3.4) Ab
Interactions between variables were significant (p < 0.001). The

PBNT
power of the multiple ANOVA was about 70%.
The two-step system SEB exhibited the highest MTBS when

–
–
–
Total-etch bonded to untreated dentin, while former prior H3 PO4 etching
decreased bond strengths, irrespective of the dentin region.
Resin–dentin bonds obtained for RES, EP, PLP, SOL and FUT

28.0 (10.2) Abc

23.5 (4.4) Ab were similar for all dentin regions and were not affected by

23.2 (5.9) Ab
acid-etching of dentin. Following H3 PO4 conditioning, MTBS
SB

to coronal dentin increased for OUB. MTBS with the total-etch

bonding agents presented similar bonding effectiveness to the

Within the same column, identical upper case letters indicate no differences (p < 0.05). For each row, matching lower case letters indicate no differences (p < 0.05).
–
–
– different dentin substrates.
Table 3 summarizes the failure modes percentage of
22.6 (11.5) Ab

17.2 (10.6) Aa

21.5 (10.5) Aa

the debonded specimens in the tested groups. Most of the

17.1 (7.0) Ab

16.8 (2.7) Aa
15.6 (4.6) Ac

observed modes of failure were adhesive. Major rates of

FUT

mixed failures were noticed for SEB groups, normally associ-

ated with higher bond strengths. Pure cohesive failures were
Table 2 – Mean microtensile bond strength (MPa) and standard deviation (S.D.) obtained for each tested group (n = 20 ± 4)

rarely detected. Root dentin showed half of the lower rate

of mixed failures when compared with the rest of dentin
22.4 (10.2) Aa
22.0 (9.9) Abc

18.2 (7.3) Abc

locations, after following the manufacturers’s directions. The

22.5 (9.7) Ab

22.1 (6.5) Ab

24.4 (5.6) Aa

percentage of mixed failures decreased after using prior H3 PO4

SOL

conditioning.
One-step self-etch

4. Discussion
25.0 (12.2) Abc

24.9 (9.4) Aab

25.4 (18.9) Ab

22.9 (11.0) Ab

21.9 (11.5) Aa
25.0 (9.8) Aa

There is a growing demand of treating cervical lesions, root

PLP

caries and root sensitivity [4,22,23]. Therefore, this study eval-

uated the effect of regional dentin variations on the MTBS of
two- and one-step self-etch bonding agents, pre-treated or not
23.6 (11.1) Bb

16.3 (10.1) Bb
23.3 (8.0) Bbc

31.5 (7.5) Aa

with 36% phosphoric acid, compared to total-etch systems.

19.7 (5.9) Ba
20.2 (6.6) Ba

The two-step self-etching system SEB exhibited the highest

OUB

MTBS when applied following manufacturer’s instructions, if

compared to the rest of the tested adhesives, irrespective of
the bonding approach (i.e., total-etch or self-etch). The supe-
rior performance of this system may be related to: (1) the
21.8 (9.0) Abc
23.0 (9.6) Ab

14.3 (5.7) Ab

18.7 (6.8) Aa
15.4 (6.4) Aa
12.9 (1.0) Ac

synergy of an unsaturated methacrylate phosphate ester (10-

MDP) as the acidic monomer in combination with HEMA [19],
EP

which is believed to improve the wetting of the tooth surface

and chelate to calcium ions of dentin [2,24]; (2) a higher expo-
sure of the peritubular dentin, which is highly mineralized
[3], bonding the specimens parallel to the tubules. This bet-
24.7 (10.3) Aa
24.1 (8.6) Abc

21.9 (9.6) Abc

18.1 (6.8) Ab

21.2 (9.4) Ab

25.7 (9.5) Aa

ter hybridization might also have been reflected in the relative

Two-step self-etch

RES

lower percentage of adhesive failures obtained after the MTBS

testing (Table 3).
H3 PO4 -conditioning produced a significantly decrease in
SEB dentin bond strength. Chelating interactions between 10-
42.7 (10.7) Aa
42.6 (13.9) Aa
40.6 (16.2) Aa
27.7 (8.7) Bab
21.2 (10.4) Ba
20.8 (8.3) Ba

MDP and dentin are reduced after phosphoric acid etching,

SEB

as hydroxyapatite crystallites availability might have further

decreased, diminishing SEB bond strength to dentin [25,26,27].
RES (two-step self-etching) yielded significantly lower
MTBS, regardless of the dentin substrate. The incorporation of
Dentin/treatment

phosphoric acid ester monomers on its formulation confers an

aggressive characteristic (pH 1) to this bonding agent, enabling
Cervical + H3 PO4
Coronal + H3 PO4

a stronger etching action on smear layers [11] and opening

Root + H3 PO4

of dentinal tubules that will produce an upward movement

Cervical
Coronal

of fluids from the underlying dentin toward the surface [18].

Root

A wet bonding technique is recommended by the manufac-

turer, so the water exudation from hydrated dentin [11,18] will
1546 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1542–1548

interfere with proper infiltration and coupling [28] of the sub-

0
4
0
sequent application of a hydrophobic rich resin (Bis-GMA and

PBNT
TEGDMA are the main components—Table 1), accounting for

49
46
40
M

–
–
–
the poor bonding performance of this adhesive.
PLP (pH 0.7), EP (pH 0.76), SOL (pH 1.8) and FUT (pH 1)

51
50
60
were neither affected by the dentin substrate nor by phospho-
ric acid etching, only OUB (pH 1.3) presented higher MTBS to

C
H3 PO4 -treated coronal dentin. Such results raise the finding

0
7
0
that within a certain range, differences in pH values may not
51
48
52
M
SB

be the only important parameter to justify differences in bond

–
–
–
strength efficiency [29]. The higher bond strengths obtained
with self-etch adhesives may also depend on other factors
A

49
45
48
[13,29], such as the dissociation constant (pKa ) [29], the chemi-
cal structure of the adhesive components (which may be more
C

0
0
0
0
0
0
or less chelating) [19], the solubility of the formed salts [24] and
FUT

its application time [6].

46
35
45
49
39
49
M

When bonding with self-etching adhesives to uncut

enamel, many manufacturers are recommending the use of
54
65
55
51
61
51
A

phosphoric acid, based upon the attained results with the

above mentioned adhesive systems, the accidental etching of
C

0
0
0
0
0
0

dentin during the adhesive procedure will not affect dentin

SOL

46
45
43
38
47
50
M

bond strength.
Moreover, it is important to stress that when one-step
54
55
57
62
53
50
A

self-etch agents are used, some problems arise: (1) a water

Adhesive system

flow-off from the bonded dentin results in a dilution of the

C

0
0
0
0
0
1

concentration of the adhesive monomers [13,30,31], lower-

ing their inward rates of diffusion; (2) the combination of
Table 3 – Distribution (as percentage) of failure modes: A: adhesive, M: mixed, and C: cohesive

PLP

48
46
48
45
44
40
M

acids, hydrophilic and hydrophobic monomers into a single

solution may compromise the function of each one of these
52
54
52
55
56
59
A

components [32,33]; (3) a differential infiltration gradient is

established as a consequence of phase separation within the
C

0
0
0
4
0
0

adhesive, and due to differences in molecular weight or affin-

ity to dentin of the infiltrating compounds of the adhesive
OUB

46
51
36
50
42
42
M

system [30,34]; (4) a relatively high concentration of solvent

is required to keep these adhesives blended in solution, and
54
49
64
46
58
58
A

air-drying is not able to accomplish significant solvent evapo-

ration [35]. The retention of water/HEMA solvents within the
C

0
2
0
0
0
0

hybrid layer hampers polymerization [36], which conducts to

reduced mechanical properties and lower bonding effective-
47
48
33
31
43
35
M
EP

ness [35,36].
Particular shortcomings related to the specific composition
53
50
67
69
57
65
A

of each one-step self-etch system may also be considered to

explain the poor bonding effectiveness obtained with these
C

0
0
0
0
0
1

adhesives. PLP and EP are solutions consisting of methacry-

late phosphoric acid mono- and di-esters, and are though to
RES

39
49
43
43
48
46
M

induce a continuous demineralization of the adjacent dentin

structures in the tubules, destabilizing the collagen [14,30]. In
61
51
57
57
52
53
A

the case of SOL, a precipitation of dissolved Ca+ salts within

the adhesive layer and the incorporation of polyetherurethane
C

5
6
8
0
0
0

(an elastomeric component with a high-molecular weight,

SEB

highly hydrophilic and hygroscopic) on its formulation may

80
64
80
65
60
59
M

have induced an osmotic water flux from deep dentin that has
also limited its bonding efficacy [33]. FUT consists of organic
15
30
12
35
40
41
A

acids combined with hydrophobic monomers and HEMA, all

dissolved in acetone. However, FUT does not contain water
Cervical + H3 PO4
Coronal + H3 PO4

on its composition, which is required to dissociate the weak

Root + H3 PO4

acids into ionized forms [11,31]. It can be assumed that its

Cervical
Coronal

acidic monomers may not be properly dissociated, resulting in

Root

lower bond strengths [31]. Its performance may also be compli-

cated by the manufacturer’s requirement of leaving the second
 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1542–1548 1547

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