Journal of Dentistry (2003) 31, 469–477

www.elsevier.com/locate/jdent

Microtensile bond strength of total-etch and

self-etching adhesives to caries-affected dentine
Laura Ceballosa, Defrén G. Camejob, M. Victoria Fuentesa, Raquel Osorioa,
Manuel Toledanoa, Ricardo M. Carvalhoc, David H. Pashleyd,*

a
Department of Dental Mater, School of Dentistry, University of Granada, Granada, Spain
b
School of Dentistry, University of Los Andes, Mérida, Venezuela
c
Department of Operative Dentistry, Endodontics and Dental Mater, Bauru School of Dentistry,
University of São Paulo, São Paulo, Brazil
d
Department of Oral Biology/Physiology, School of Dentistry, Medical College of Georgia, Augusta,
GA 30912-1129, USA

Received 4 April 2003; accepted 24 April 2003

KEYWORDS
Dentine bonding; Total-
etch; Self-etch; Caries-
affected dentine;
Microtensile bond
strength; Microhardness;
DIAGNOdent laser
Summary Objectives. To evaluate the microtensile bond strength of total-etch or self-
etch adhesives to caries-affected versus normal dentine, and to correlate these bond
strengths with DIAGNOdent laser fluorescence and Knoop microhardness (KH)
measurements of the substrates.
Methods. Extracted carious human molars were ground to expose flat surfaces
where the caries lesion was surrounded by normal dentine. Surfaces were bonded with
either Prime & Bond NT, Scotchbond 1, Clearfil SE Bond or Prompt L-Pop, according to
manufacturers’ recommendations. A crown was built up using resin composite (Tetric
Ceram). After storage in water (37 8C, 24 h), teeth were vertically serially sectioned
into 0.7 mm thick slabs and trimmed to yield 1 mm2 test area that contained either
caries-affected or normal dentine. Samples were tested in tension in an Instron
machine at 1 mm/min. The quality of the dentine just beneath each fractured
specimen was measured by laser fluorescence and KH.
Results. Total-etch adhesives yielded higher bond strengths than self-etching
systems. Significantly lower results were obtained with Prompt L-Pop. All the
adhesives attained higher strengths in normal than in caries-affected dentine, but
the differences were only significant for Prime & Bond NT and Clearfil SE Bond. Higher
laser fluorescence values and lower KH ðp , 0:001Þ were recorded in caries-affected
dentine compared to normal dentine.
Conclusions. The total-etch adhesives evaluated produced higher bond strengths to
normal and caries-affected dentine than self-etching systems. Laser fluorescence
measurements discriminated caries-affected dentine from normal dentine, and were
strongly correlated with KH. However, laser fluorescence and KH did not permit high
correlations with resin-dentine bond strengths in caries-affected dentine.
Q 2003 Elsevier Ltd. All rights reserved.

Introduction
*Corresponding author. Tel.: þ1-706-721-2033; fax: þ1-706-
721-6252. The infiltration of resin monomers within the
E-mail address: dpashley@mail.mcg.edu demineralized microporous collagen fibril scaffold

0300-5712/03/$ - see front matter Q 2003 Elsevier Ltd. All rights reserved.
doi:10.1016/S0300-5712(03)00088-5
470
to establish a hybrid layer, and the formation of
resin tags that seal the opened tubules constitute
the major and most effective ways to bond resins to
dentine.1 – 3 A number of new adhesive systems have
been developed in an attempt to reduce the steps
and simplify clinical bonding procedures. Two
major simplified bonding approaches have been
developed.4 The first utilizes the total-etching
technique to simultaneously remove the smear
layers from both enamel and dentine surfaces,
followed by the application of a one-bottle agent
that combines the primer and the adhesive in one
solution.5 As the demineralized collagen fibril mesh
is used as the bonding substrate, a wet bonding
technique is required to insure its full expansion.6,7
The need for a moist dentine surface in complex
cavity preparations often create overwet and
underwet regions in the same tooth, making
bonding to dentine with these adhesives very
technique sensitive.8 – 10
The second approach is the use of self-etching
primers.4,11 Their bonding mechanism is based
upon the simultaneous etching and priming
of the smear-covered dentine using an acidic
primer,12,13 followed by the application of an
adhesive resin. Self-etching primers eliminate the
separate acid-etching and rinsing steps, simplifying
bonding technique and reducing its technique-
sensitivity.10,14,15
Recently, all-in-one adhesive systems have been
also introduced to simplify the bonding procedure
even more. These are also named self-etching
adhesives and combine the etching, priming and
bonding procedures into one solution and one
step.14
The efficiency of these simplified bonding
systems is still controversial4 and practically all
published reports used normal dentine as the
bonding substrate. However, most clinical adhesive
procedures involve altered forms of dentine, such
as sclerotic or caries-affected dentine.16,17 The
development of the microtensile test method, that
utilizes specimen cross-sectional areas of approxi-
mately 1 mm2, has allowed the determination of
bond strengths of several bonding systems to caries-
affected dentine.16,18 – 21 Previous studies have
reported that the bond strengths of self-condition-
ing systems seems to be markedly reduced on
caries-affected dentine.18,21,22 . However, the
adhesive properties of the new, all-in-one systems
to caries-affected dentine have not yet been
extensively reported.
According to this method,16 after conducting the
bond strength testing, the quality of the caries-
affected dentine, previously defined by combined
criteria of visual examination and staining by
L. Ceballos et al.
a caries detector solution, is confirmed by measur-
ing the Knoop hardness of the substrate. It has been
demonstrated that microhardness measurements
correlate well with the degree of mineralization,23
with caries-affected dentine being significantly
softer than normal dentine.16,18,19,24 – 26 However,
this technique is time-consuming and requires the
use of a microhardness tester, which is not
available in most laboratories.
New non-invasive, optical instrument-based
techniques for detection and quantification of
demineralization have been recently developed.27
One example is the introduction of a device called
the DIAGNOdent, based on the fluorescence of
tooth structure when teeth are illuminated with a
laser light (l ¼ 655 nm). This radiation is absorbed
by both inorganic and organic tooth substance28 and
by metabolites from oral bacteria.29 Emitted
fluorescence is observed through a high-pass barrier
filter that discriminates between sound and carious
tissue. 30 If there is a significant relationship
between Knoop hardness values and the fluor-
escence values of the DIAGNOdent, the latter
device might be more convenient to estimate the
quality of the caries-affected dentine in microten-
sile bond test studies.
The aim of the present study was to evaluate the
microtensile bond strength of two total-etch and
two self-etching adhesive systems to normal and
caries-affected dentine, and to compare DIAGNO-
dent laser fluorescence and Knoop microhardness
measurements to quantitate the degree of demi-
neralization of caries-affected dentine following
resin-bonding. Two hypotheses were tested. The
first hypothesis is that the bond strengths of
adhesive systems to caries-affected dentine is
lower than to normal dentine. The second is that
the more carious the dentine (i.e. the softer or
more demineralized the dentine), the lower will be
its bond strength.
Materials and methods
Specimen preparation
Sixteen extracted human molars with coronal
dentine caries extending approximately halfway
through the dentine were used in this study. All
teeth had been stored at 4 8C in physiological saline
to which several crystals of thymol were added.
Specimens were prepared as described by Nakajima
et al.16 to perform microtensile bond strength tests
on caries-affected dentine. Occlusal surfaces were
ground perpendicular to the long axis of the tooth
Microtensile bond strength of total-etch and self-etching adhesives to caries-affected dentine 471

with #220 silicon carbide paper under running water
(EXAKT- Apparatebau D-2000 Nerderstedt,
Germany) to expose a flat surface where the caries
lesion was surrounded by normal dentine. To obtain
caries-affected dentine, the samples were ground
using the combined criteria of visual examination
and staining with 0.5% fucsin dye, until relatively
hard, non-staining dentine was obtained. Four
teeth were randomly allocated to each of the four
treatment groups.
Bonding procedure and bond strength
testing
Four different adhesive systems were applied
following the manufacturers’ recommendations
(Table 1). Two were total-etch, one-bottle
adhesives: Prime & Bond NT (Dentsply DeTrey,
Konstanz, Germany) and Scotchbond 1 (3M-ESPE,
St Paul, MN, USA); and two more were self-etching
systems: Clearfil SE Bond (Kuraray Co. Ltd., Osaka,
Japan) and the all-in-one adhesive system, Prompt
L-Pop (3M-ESPE, St Paul, MN, USA). A composite
crown was built up by applying several layers of
Tetric Ceram (Ivoclar-Vivadent, Schaan, Liechten-
stein) hybrid resin composite to a height of 3 –5 mm.
Each increment was cured for 40 s. The teeth were
stored in water at 37 8C for 24 h and then vertically
serially sectioned perpendicularly to the bonded
interface to produce several bonded sections of
approximately 0.7 mm thick (Accutom-50, Struers,
Copenhagen, Denmark).
Each slice was carefully examined to separate
those that contained caries-affected dentine from
those containing normal dentine, following the
visual criterion described above. About three slabs
of normal dentine and two to three slabs of caries-
affected dentine were obtained per tooth (10 per
group). All the slabs were trimmed to yield
an hourglass shape with a 1 mm2 test area that
contained either caries-affected or normal
dentine.

Table 1 Dentine adhesive systems tested.

Adhesive system Principle ingredients Mode/steps of application

Prime & Bond NT PENTA, UDMA resin, Resin R5-62-1, Etch for 15 sec with 35% phosphoric
(Dentsply De Trey T-resin, D-resin, nanofiller, initiators, acid. Rinse with water for 15 s
GmbH, Konstanz, stabilizer, cetylamine hydrofluoride, and remove excess water with 1 s
Germany) acetone air blast. Apply ample adhesive to
saturate moist surface, reapply if
necessary. Leave surface undisturbed
for 20 s; Remove solvent gently with
air for 5 s. Light-cure 10 s
Scotchbond 1 Bis-GMA, HEMA, dimethacrylates, Etch 15 s with 35% phosphoric acid.
(3M, St Paul, MN, USA) polyalkenoic acid copolymer, Rinse with water for 10 s. Apply two
initiator, water, ethanol consecutive coats of the adhesive
to moist dentine with a saturated
brush tip. Dry gently for 2–5 sec;
Light cure 10 s

Clearfil SE Bond Primer. 10-methacryloyloxydecyl Apply Primer for 20 s;

(Kuraray Co, Osaka, Japan) dihydrogen phosphate; Evaporate water with mild air;
2-hydroxyethyl methacrylate; hydrophilic Apply adhesive, Gentle air
dimethacrylate; dl-camphorquinone; stream. Light cure 10 s
N,N-diethanol-p-toluidine; water
Adhesive. 10-methacryloxydecyl
dihydrogen phosphate;
Bis-phenol A diglycidylmethacrylate;
2-hydroxyethyl methacrylate;
hydrophobic dimethacrylate;
di-camphorquinone;
N,N-diethanol-p-toluidine;
silanated colloidal silica
Prompt L-Pop Water, methacrylated phosphoric Apply with scrubbing
(3M-ESPE, St Paul, acid esters, phosphine oxide, for 15 s. Gently air dry,
MN, USA) stabilizer, zinc fluoride complex, Light cure 10 s
parabenes
472
Samples were attached to a Bencor Multi-T
testing apparatus with a cyanoacrylate adhesive
(Zapit, DVA, Anaheim, CA, USA) and subjected to
tensile stress in an universal testing machine (Model
4411, Instron Corp., Canton, MA) at a cross-head
speed of 1 mm/min until failure. The bond
strengths were expressed in MPa after measuring
the cross-sectional area at the site of fracture with
a digital caliper (Mitutoyo, Tokyo, Japan).
DIAGNOdent laser and microhardness
measurements:
After performing the microtensile test, the lateral
aspect (i.e. the non-bonded surface) of each
dentine-half of the fractured specimens was highly
polished with #4000 silicon paper in a circular
grinding machine (EXAKT-Apparatebau D-2000 Ner-
derstedt, Germany) to permit subsequent micro-
hardness measurements.
Prior to microhardness measurements, the
degree of demineralization of the specimen was
measured with the laser fluorescence system
(DIAGNOdent, KaVo, Biberach, Germany). Before
the start of the measurements, the laser was
calibrated against a porcelain standard as indicated
in the manufacturer’s instructions. The measure-
ments were performed using the smallest conical
tip (1.2 mm diameter) that was held against the
specimen at right angles to the surface. The
maximum fluorescence reading was recorded just
beneath the fractured site. Progression of the
carious process is reflected in an increase in the
amount of fluorescence.31 The numerical range of
the DIAGNOdent instrument is from 0 to 100.
Finally, Knoop microhardness measurements
were done 50 mm below the adhesive/dentine
interface using an Instron Wolpert hardness tester
(V-testor 4021, Instron Wolpert GmbH, Ludwgsha-
fen, Germany), under a load of 30 g and a duration
of 30 s. During the test, dentine desiccation was
Table 2 Mean microtensile bond strengths (MPa) and standard deviation (SD) to normal and caries-affected dentine.
Adhesive system Normal dentine
Prime & Bond NT 56.3 (11.1) a
Scotchbond 1 43.9 (11.4) b
Clearfil SE Bond 35.5 (11.6) b
Prompt L Pop 18.2 (9.6) c
For each column, means designated by the same letter are not significantly different ðp . 0:05Þ: NS: not significantly different.
Values are mean ^ SD in MPa.
a
Shows statistical differences between normal and caries-affected dentine ðp , 0:05Þ:
L. Ceballos et al.
avoided.32 Each specimen received approximately
five indentations and were averaged.
Statistical analysis
A two-way ANOVA was performed to evaluate the
effect of the adhesive and the type of dentine
tested, and their interactions, on microtensile bond
strength. Statistical significance was set in advance
at the 0.05 probability level. Multiple post-hoc
comparisons were done using Student-Newman –
Keuls test.
Comparison of the values obtained by either
laser fluorescence or microhardness tests, on
normal dentine and caries-affected dentine were
performed by Student’s t test. The correlation
between laser fluorescence values and Knoop
microhardness numbers, as well as the correlations
between microtensile bond strength and fluor-
escence values and between bond strength and
microhardness measurements were analyzed by
calculating Pearson’s correlation coefficient. All
data were analyzed by means of SPSS 10.0 for
Windows software (SPSS Inc., Chicago, IL, USA).
Results
The results of microtensile bond strength test are
shown in Table 2. Two-way ANOVA revealed a
significant influence of both the adhesive systems
tested ðF ¼ 40:857; p , 0:0001Þ and the type of
dentine ðF ¼ 22:088; p , 0:0001Þ on microtensile
bond strength values. However, the interaction of
these two factors was not statistically significant
(F ¼ 1.282; p ¼ 0.287).
ANOVA analysis showed significant differences
among the adhesive systems evaluated for normal
ðF ¼ 21:892; p , 0:0001Þ and caries-affected den-
tine ðF ¼ 23:701; p , 0:0001Þ: In normal dentine,
Prime & Bond NT attained the highest micro-
tensile bond strength. Intermediate, statistically
similar bond strengths were obtained in normal
Sig. Caries-affected dentine
,0.05a 41.3 (10.7) A
NS 36.3 (12.2) A
,0.05a 21.5 (5.5) B
NS 13.4 (1.9) C
Microtensile bond strength of total-etch and self-etching adhesives to caries-affected dentine
Table 3 Failure modes for the adhesives in normal and caries-affected dentin.
Adhesive system Adhesive
Prime & Bond NT
Normal dentine 10%
Caries-affected dentine 33.3%
Scotchbond 1
Normal dentine 25%
Caries-affected dentine 71.4%
Clearfil SE Bond
Normal dentine 46.7%
Caries-affected dentine 63.6%
Prompt L-Pop
Normal dentine 100%
Caries-affected dentine 90%
dentine with Scotchbond1 and Clearfil SE Bond,
while Prompt L-Pop showed the lowest strengths
(Table 2). In caries-affected dentine, the total-
etch adhesive systems, Prime & Bond NT and
Scotchbond 1, yielded statistically higher ðp ,
0:05Þ bond strengths than Clearfil SE Bond.
Significantly lower ðp , 0:05Þ strengths were
obtained with Prompt L-Pop.
In normal dentine, the major mode of failure in
specimens showing low bond strengths was adhesive
failure, while cohesive fractures in dentine or
composite were seen at higher bond strengths
(Table 3). In caries-affected dentine, adhesive and
cohesive failures in dentine were seen in specimens
showing low bond strengths, while cohesive failures
in resin composite were seen more frequently in
specimens with high bond strengths.
All the adhesives tested showed higher strengths
in normal dentine than in caries-affected, but these
differences were only significant for Prime & Bond
NT and Clearfil SE Bond.
The results of laser fluorescence and Knoop
hardness numbers for normal and caries-affected
dentine are shown in Table 4. Significantly lower
fluorescent values were obtained for normal den-
tine ðt : 19:289; p , 0:0001Þ; compared with the
values recorded in caries-affected dentine. Mean
hardness results for normal dentine were statisti-
cally significant higher ðt : 17:495; p , 0:0001Þ than
those of caries-affected dentine. Comparison
between laser fluorescence values recorded and
Knoop hardness numbers (KHN) of all of the speci-
mens (Fig. 1) revealed a high correlation
ðr ¼ 20:85; p , 0:0001Þ:
However, the correlation between all resin-
dentine bond strengths and fluorescence values
473
Cohesive in dentine Cohesive in composite
10% 80%
33.3% 33.3%
12.5% 62.5%
14.3% 14.3%
13.3% 13.3%
36.4% 0
0 0
10% 0
was low (r ¼ 20:334; data not shown) but was
significant ðp , 0:01Þ: Similarly, the correlation
between microtensile bond strength and KH values,
while significant ðp , 0:001Þ; was low (r ¼ 0:412;
data not shown). These correlations were done
excluding the specimens bonded with Prompt L-
Pop, as the bond strengths attained with this
adhesive were so low. Thus, the potential utility
of using KHN or fluorescence values for predicting
bond strength using all combined types of dentine is
poor. If the correlation of bond strength and KHN
is limited to caries-affected specimens, then the
correlation becomes even weaker ðr ¼ 0:119;
p ¼ 0:554Þ: Similarly, the correlation between
bond strengths of caries-affected dentine and
fluorescence values was insignificant (r ¼ 20:023;
p ¼ 0:90 data not shown).
When these correlations were done for each
adhesive separately, they were not significant for
Scotchbond 1 or for Prompt L-P. However, the
correlation between bond strength and KH for
Prime & Bond NT was moderate ðr ¼ 0:548;
p , 0:05Þ and the same was observed for Clearfil
SE Bond ðr ¼ 0:472; p , 0:01Þ: Similarly, the corre-
lations between bond strength and fluorescence
Table 4 DIAGNOdent values and Knoop microhardness
numbers obtained in normal and caries-affected dentine.
DIAGNOdent Knoop microhardness
values number
Normal dentine 8.5 (12.6) a 74.6 (9.1) A
Caries-affected dentine 61.6 (20.9) b 33.9 (6.7) B
For each column, values with different letters indicate
statistically significant difference ðp , 0:05Þ:
474
Figure 1 Correlation between Knoop hardness values and DIAGNOdent fluorescent values on the same specimens.
values for Prime & Bond NT and Clearfil SE Bond
were also relatively low, but were significant
(r ¼ 20:49; p , 0:05 and r ¼ 20:514; p , 0:01;
respectively).
Discussion
The results of the present study show that bond
strength to normal and caries-affected dentine is
dependent on the adhesive system used. In normal
dentine, the total-etch adhesives tended to pro-
duce higher bond strength values than the self-
etching adhesives, confirming the observations of
Inoue et al.33
Prime & Bond NT exhibited the highest bond
strengths compared with the other total-etch
adhesive, Scotchbond 1. Prime and Bond is filled
with nanoparticles that may help to establish a
thicker more uniform resin film thickness that
stabilizes the hybrid layer,14 although this effect
is still somewhat controversial.34,35
The lowest microtensile bond strengths were
attained with Prompt L-Pop, that exclusively
yielded adhesive failures. These results are in
agreement with previous reports that this product
produces inconsistent results.11,14,36,37 Prompt L-
Pop produces an etching pattern similar to phos-
phoric acid, being classified as a strong self-etching
adhesive, in contrast with the mild etching ability
of Clearfil SE Bond.14,15 Both bonding systems form
authentic hybrid layers. However, Prompt L-Pop
dissolves the smear layer and plugs while Clearfil SE
L. Ceballos et al.
Bond preserves and incorporates them into the
hybridized complex.15 This etching aggressiveness
is unrelated to the bond strengths attained.11 One
explanation may be the formation of dry spots
where the low viscosity Prompt L-Pop had spread so
thin that it may not be properly polymerized.36,37
Higher strengths have been reported for this
adhesive when it is applied in multiple coats38 or
is experimentally filled.36,37
In caries-affected dentine, the total etch
adhesives performed better than the self-etching
systems. Caries-affected dentine contains dentinal
tubules that are filled with acid-resistant whitlock-
ite minerals25,39,40 – 42 that interfere the infiltration
of adhesive resins and the formation of resin
tags.42,43 The application of 32 – 37% phosphoric
acid seems to solubilize the intratubular mineral
deposits in caries-affected dentine19 – 21 better than
weaker acids, thereby contributing to better resin
retention.3 It may be that Clearfil SE Bond is not
acidic enough to dissolve the mineral casts. More-
over, the smear layer formed on caries-affected
dentine includes acid resistant crystals that may
hamper the diffusion of the self-etching primer into
the underlying intact dentine.21 However, since the
presence of these deposits in dentinal tubules has
been shown to reduce dentine permeability44 to
near zero and hence constitutes a protective
barrier for the pulp tissue by reducing the ingress
of bacteria, and/or bacterial products,40,42 it
should be retained in conservative cavity prep-
arations,42 as it is generally not infected and can
remineralize.45
Microtensile bond strength of total-etch and self-etching adhesives to caries-affected dentine
The low bond strengths produced by Prompt L-
Pop may not be related to its etching aggressiveness
but to its degree of conversion. All-in-one systems
do not yet possess all the requirements to provide
optimal adhesion to tooth structure.11 Modifi-
cations in its formulation or mode of application
are needed.36 – 38 It is noteworthy that Prompt L-Pop
has been ported to be relatively ineffective in
retention of resin composite restorations to non-
carious cervical sites in a clinical trial.46
Caries-affected intertubular dentine is partially
demineralized due to the caries process,25,41,44 and
is more porous, allowing deeper penetration of
monomers.22 This fact is reflected in the establish-
ment of thicker hybrid layers.16,18 – 22 However, the
thickness of the hybrid layer is unrelated to bond
strengths in dentine.16,18 – 22 Even when the adhesive
systems are capable of infiltrating deep into inter-
tubular dentine, there would be always a porous and
demineralized underlying zone that was not infil-
trated.42 Moreover, caries-affected dentine pre-
sents lower nanomechanical properties44 and a
lower cohesive strength22 (Fuentes, unpublished
observations) as they are dependent on the proper-
ties of intertubular dentine.47 Thus, the weakest link
in the resin-caries-affected dentine assembly may
be the cohesive strength of caries-affected dentine.
Knoop hardness testing revealed the caries-
affected dentine to be about half as hard as
normal dentine, in agreement with previously
reported results.16,18 – 20,25 This relative softness
of caries-affected dentine is due to the partial
demineralization of the intertubular dentine even
though tubules become filled with mineral.16,25,48
In the present study, lower Knoop hardness values
in caries-affected dentine were strongly corre-
lated with higher laser fluorescence values (Fig. 1),
confirming the results of Banerjee et al.49 There-
fore, these results reveal the capacity of the laser
fluorescence device to estimate the quality of
caries-affected dentine relative to normal den-
tine. Its non-destructive nature, in addition to its
repeatability and validity have been claimed to
make it an useful tool in a clinical and laboratory
situation.30,50 – 53 The mechanism underlying the
enhanced fluorescence in the presence of caries
has not been fully clarified.54 Unlike Knoop
hardness,23 no relationship between autofluores-
cence and the mineral content of caries lesions
has been found. This may be due to the
contribution of exogenous fluorescent molecules
imported during the carious process.55
The DIAGNOdent instructions describe a scale
which correlates the numerical values with histo-
logical findings, and provide treatment rec-
ommendations. However, this scale makes no
475
distinction between acute or active carious lesions
versus chronic or arrested lesions. Moreover, it
has been reported that high laser fluorescence
readings may also be obtained on dentine surfaces
which are stained.51,56 It must be borne in mind
that caries-affected dentine presents a glassy,
dark yellow or slightly brown appearance. This
may produce higher DIAGNOdent scores49,56 than
less colored caries lesions with the same degree
of demineralization. This potential source of error
of DIAGNOdent has been previously be pointed out
to be a distinct disadvantage,57 compared with
the visual system, as laser fluorescence system
can only detect carious lesions but cannot judge
their activity.51
In caries-affected dentine, the relationship
between bond strength and hardness or fluor-
escence values were not significant when all the
specimens were considered. Even using the
smallest laser probe, the DIAGNOdent sampled
an area of about 1 mm2 or a volume **(for a
0.7 mm thick specimen) of 0.7 mm3 that was
located subjacent to the bonded surface area.
That is, it only gives an average fluorescence
value of dentine at some distance below the
bonded surface. Fig. 1 shows that the fluor-
escence values varied from 35 to 98 in caries-
affected dentine, yet the resin-dentine bond
strengths did not vary as much as the fluorescence
values (data not shown). Although the KH numbers
were also measured below the bonded surface, it
was only 50 mm below, instead of 500 mm or more
as was the case with the DIAGNOdent. The Knoop
hardness measurements are made with a large
indenter that crushes both intertubular and
peritubular dentine. That is, it measures an
average hardness. In caries-affected dentine, the
tubules are filled with mineral crystals that
prevent resin tag formation and make these
tubules harder than fluid-filled tubules.44 Dentine
bond strengths under these conditions are prob-
ably due to hybridization of intertubular den-
tine.58 Better correlations between bond strengths
and hardness of caries-affected dentine may
require use of nanohardness techniques.4,43
Conclusions
All the adhesives evaluated in the present study
showed higher strengths to normal dentine than in
caries-affected, but these differences were only
significant for Prime & Bond NT and Clearfil SE
Bond. The occlusion of dentinal tubules by the acid-
resistant mineral deposits that interferes with
476
the formation of retentive resin tags and the
intrinsic weakness of caries-affected dentine may
have contributed these results. In caries-affected
dentine, total-etch adhesives performed better
than self-etching systems.
Higher laser fluorescence values were strongly
correlated with lower Knoop hardness values in
caries-affected dentine. Thus, although both the
DIAGNOdent and KH values correlate well to each
other and can measure differences in the quality of
dentine, the regions that they sample may be too
far removed from the resin-dentine interface to
permit high correlations with resin-dentine bond
strengths.
Acknowledgements
This research project was supported by grant
DEO14911 from the National Institute of Dental
and Craniofacial Research, by grant MAT
2001-2843-CO2; RED CYCTED VIII.J. from the
CICYT, Spain. The authors wish to thank Gertrudis
Gómez-Villaescusa for her help with specimen
preparation.
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