journal of dentistry 38 (2010) 480489

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An in vitro evaluation of microtensile bond strengths of two

adhesive bonding agents to residual dentine after caries
removal using three excavation techniques
A. Banerjee *, S. Kellow, F. Mannocci, R.J. Cook, T.F. Watson
Kings College London Dental Institute, KCL, United Kingdom

article info

abstract

Article history:

Objectives: To assess amounts of residual dentine retained after using three excavation

Received 21 January 2010

techniques; the microtensile bond strengths (mTBS) to residual dentine, comparing etch-

Received in revised form

rinse vs. self-etching adhesives.

22 February 2010

Methods: 42 carious molars were subdivided (N = 21) dependent upon adhesive/composite

Accepted 2 March 2010

system (Adper Scotchbond 1XT and Filtek Supreme vs. Filtek Silorane adhesive and composite). Dividing into three (N = 7), dependent upon caries excavation technique employed
(hand vs. chemo-mechanical: CarisolvTM gel vs. experimental enzymatic gel (SFC-V)), caries

Keywords:

removal was assessed using visual/tactile criteria and in situ autofluorescence (AF) confocal

Dentine

fibre-optic micro-endoscopy (CFOME). Post-restoration/four-week hydrated storage, four

Caries

0.9 mm2 beams per tooth underwent mTBS testing/microscopic analysis of fractured sur-

Excavation

faces. Three cavities from each excavation group were analysed using SEM.

Microtensile bond strength

Results: SEM revealed surface roughness with smear layer occluding tubule orifices in hand-

Dentine bonding agent

excavated samples and a reduced, variable smear layer for both chemo-mechanical sys-

Confocal microscopy

tems. CFOME AF assessment indicated hand excavation left sound dentine, CarisolvTM left

Composite

affected dentine and SFC-V slightly under-prepared clinically. Mean mTBS values from etch-

Silorane

rinse samples (27 MPa (SD 3.9), hand; 22 MPa (SD 5.1), CarisolvTM; 26 MPa (SD 4.4), SFC-V)

Carisolv

TM

gel

showed statistical differences between hand and CarisolvTM groups. Mean mTBS data for
self-etch samples (22 MPa (SD 3.3), hand; 27 MPa (SD 6.1), CarisolvTM; 25 MPa (SD 4.7), SFC-V)

Biosolv

showed significant differences between hand and CarisolvTM, and hand vs. SFC-V. Failure
loci distribution in etch-rinse samples was between dentineadhesive, within adhesive and
within composite whereas self-etch samples exhibited failure predominantly between
adhesive and composite.
Conclusions: Data indicated that all null hypotheses were disproved.
# 2010 Elsevier Ltd. All rights reserved.

1.

Introduction

The increasing evidence and popularity of the minimally

invasive operative management of carious dentine has brought
into question the apparent necessity for complete caries

removal when restoring a cavitated lesion in a patient.1,2 The

superficial necrotic zone of caries-infected dentine that
harbours the core bacterial biomass should be excavated
leaving only residual caries-affected dentine lining the
cavity with sound enamel margins and dentine adjacent to the

* Corresponding author at: Kings College London Dental Institute, KCL, Floor 26, Tower Wing, Guys Dental Hospital, London Bridge,
London. SE1 9RT. Tel.: +44 0207 188 1577 7486; fax: +44 0207 188 1577 7486.
E-mail address: avijit.banerjee@kcl.ac.uk (A. Banerjee).
0300-5712/$ see front matter # 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jdent.2010.03.002

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journal of dentistry 38 (2010) 480489

enameldentine junction (EDJ).3,4 This will enable the best

peripheral seal to be achieved with the current adhesive
dentine bonding systems, as long as sufficient moisture
control can be obtained.
Identification of the histological transition zone between
infected and affected dentine is difficult to assess both
clinically and in the research laboratory. Change in colour is
not a good indicator as the gradual bacterial and histological
changes are not consistently colour-dependent.5 Caries
detector dyes based on propylene glycol were developed in
order to highlight alterations in dentine collagen structure but
publications have shown that clinical and laboratory results
produced are open to considerable user-interpretation.68 The
relative hardness/tactility of the dentine has clinical validity;9
sound dentine is scratchy to a sharp dental explorer, infected
dentine has a soft, mushy consistency and affected dentine
falls in between, often simultaneously scratchy and tacky, but
again this method of identifying the transition zone is fraught
with operator subjectivity.4 The autofluorescence (AF) of
carious dentine has been proposed as a potential marker for
that carious dentine requiring excavation but originally, the
confocal microscopy equipment used to detect the AF
signature could only be useful in laboratory research experiments where extracted tooth sections could be prepared.1013
More recently, this technology has been developed into a
confocal fibre-optic micro-endoscope (CFOME) which can
operate in situ during active caries excavation in whole teeth,
so providing immediate numerical, objective feedback of the
AF quality of the residual carious dentine.14
The selective removal of caries-infected dentine is not
easily achieved with the most popular current operative caries
excavation techniquesthe rotary bur and spoon-shaped hand
excavator. This is due to their relative tactile insensitivity and
operator variability in use leading to varying quantities of
tissue removed.13 Chemo-mechanical agents have been
developed to be used in conjunction with their own hand
instruments and evidence exists to show that their careful use
may offer some element of selectivity between the infected
and affected dentine. One such gel system currently available
for clinical use is based upon the controlled activity of sodium
hypochlorite on dentine collagen, used with abrasive hand
instruments (CarisolvTM gelOraSolv AB, Gothenburg, Sweden).13,15 Another, based upon the enzymatic action of pepsin
in an acidic environment (SFC-V, Biosolv, 3MESPE AG,
Seefeld, Germany) is at the clinical trial phase of its

development but shows promise. Another factor to consider

in terms of restoring the resulting cavity with adhesive
materials, is the final dentine surface characteristics (surface
roughness, presence of smear layer) which can affect the final
bond and seal achieved by adhesive systems.16,17
In terms of factors affecting the long term success of
adhesive restorations, the marginal integrity/potential for
microleakage at the tooth-restoration interface due to a poor
seal, appear high on the list.18,19 This in turn is closely
associated with the quality of the bond achieved by modern
dentine bonding systems. Current adhesives tend to fall
broadly into one of two groupsthe etch-and-rinse systems
which involve a separate etch phase with 37% orthophosphoric acid on both enamel and dentine for approximately
20 s prior to placement of the primer and bond (adhesive), or
the self-etching systems which incorporate the acidic moieties within the primer phase of the bonding system, which
are incorporated into the final adhesive layer. There is
evidence extolling the potential virtues of each system in
the strength of the bond achieved to varying dental substrates,2022 but less conclusive evidence when specifically
considering the bond to caries-affected dentine.21,2329
Therefore the null hypotheses to be investigated in this
study were:
1. There are no differences in the amount and quality of
carious dentine excavated by three different clinical hand
excavation techniques (CarisolvTM gel, SFC-V and hand
excavation).
2. Using three different caries excavation techniques (CarisolvTM gel, SFC-V and hand excavation) has no effect on
adhesive bond strengths to the residual carious dentine,
comparing total-etch and self-etching dentine bonding
systems.
3. Using three different caries excavation techniques (CarisolvTM gel, SFC-V and hand excavation) has no effect on the
failure mode and loci of failure when bonding to the
residual carious dentine, comparing total-etch and selfetching dentine bonding systems.

2.

Materials and methods

The materials used in this study are outlined in Table 1. With

Guys Hospital research ethics approval (04/Q0704/57), 51
extracted, human cavitated carious molars, stored in water for

Table 1 Materials used in the study.

Brand name

Manufacturer

Batch no.

Adper Scotchbond 1XT

Filtek Supreme
Filtek Silorane adhesive
Filtek Silorane
CarisolvTM gel

3MESPE AG, Germany

3MESPE AG, Germany
3MESPE AG, Germany
3MESPE AG, Germany
Orasolv AB, Sweden

20050711
20030322
Experimental sample
203905
06009

SFC-V (Biosolv)

3MESPE AG, Germany

0540

Type/constituents
Total-etch dentine bonding agent
Hybrid resin composite
Self-etch dentine bonding agent
Low-shrink siloxaneoxirane composite
Chemo-mechanical caries removal gel
(0.5%, w/v sodium hypochlorite; 0.1 M
glutamic acid/leucine/lysine, sodium
chloride, sodium hydroxide,
carboxymethycellulose
Experimental chemo-mechanical caries
removal gel (pepsin, phosphoric acid/sodium
biphosphate buffer)

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journal of dentistry 38 (2010) 480489

no longer than four weeks, were selected and 42 of these were

randomly divided into two experimental groups (N = 21),
according to the type of adhesive restorative system used.
Teeth in one group would be restored using an etch-and-rinse
bonding agent plus a nano-hybrid resin composite (Adper
Scotchbond 1XT with Filtek Supreme resin composite
(3MESPE, Seefeld, Germany)) whilst those in the other would
be restored with self-etching Filtek Silorane bond and lowshrink Filtek Silorane composite (see Table 1). Each of these
groups was further subdivided into three subsets, dependent
upon the caries excavation technique employed: conventional
hand excavation using a spoon-shaped hand excavator,
CarisolvTM gel and SFC-V Biosolv (N = 7 in each).

become cloudy with a muddy consistency, it was rinsed

away and a second fresh mix of gel was applied and further
agitated. Excavation was deemed complete when the gel failed
to become cloudy and the cavity was checked with a dental
probe for hardness. The remaining seven teeth in each group
underwent chemo-mechanical caries removal using SFC-V
solution, with the same mace-tip instrument. The SFC-V was
introduced into the cavity and was immediately agitated using
the mace-tip hand instrument and washed away with further
subsequent applications until the gel did not remove any
further dentine and did not become turbid (see Fig. 2).

2.1.

The remaining nine teeth with cavitated occlusal caries were

subdivided into three groups (N = 3) according to the caries
excavation technique employed (see above). After excavation,
rinsing and drying the final cavities, addition-cured light body
silicone impressions were taken (President, Coltene AG,
Switzerland) and from these, epoxy resin replicas created,
gold sputter-coated and imaged using SEM (Hitachi S520Hitachi Scientific Instruments, Wokingham, Berks., UK),
12 kV).

Caries excavation

Under 3 magnification dental loupes, a tungsten carbide

fissure bur in an air-turbine handpiece (No. 57, Smartbur,
Bridgewater Corners, USA) was used to remove any overlying,
undermined enamel, so exposing the full extent of occlusal
carious dentine including a periphery of sound dentine. Seven
teeth from each of the two main groups underwent clinical
caries excavation using a spoon-shaped hand excavator, using
operator-dependent tactility to determine the endpoint of
caries excavation (see Fig. 1). A separate seven teeth in each
group underwent caries excavation using CarisolvTM gel as per
manufacturers instruction, using an abrasive metal mace-tip
instrument provided. The pre-mixed gel was introduced into
the cavity for 40 s prior to agitating the mixture against the
dentine using the mace-tip instrument. Once the gel had

2.2.

2.3.

Scanning electron microscopy (SEM)

CFOME AF measurements

The confocal laser imaging system (Cellvizio1 Mauna Kea

Technologies, Paris, France) was configured with a 600 mm
diameter plane-ended mini-o1 surface contact optical fibre
bundle objective probe (015 mm focal plane depth, <5 mm

Fig. 1 Caries excavation using a spoon-shaped hand excavator. (a) Original cavitated mandibular molar, (b) carious dentine
with peripheral sound dentine exposed after enamel removal, (c) infected dentine excavated with hand instrument, and (d)
completed caries excavation with scratchy sound dentine remaining.

journal of dentistry 38 (2010) 480489

483

Fig. 2 Caries removal using chemo-mechanical CarisolvTM gel. (a) The original occlusally cavitated carious lesion in a
mandibular molar. (b) The full extent of the carious dentine and sound margin exposed after enamel removal. (c) Clear gel
applied and left for 40 s before (d) agitation against the dentine using a mace-tip abrasive hand instrument. (e) Turbidity of
the gel prior to rinsing and (f) the final excavation when no further caries is dissolved by the gel, leaving affected dentine.

lateral resolution, approximately 15 mm axial resolution and

no distal optical element). After enamel preparation, the preexcavation autofluorescence of the carious dentine in all
samples was recorded using 488 nm laser illumination. AF
wavelengths, detected via the same coherent fibre elements,
were delineated from reflected illumination wavelengths
using >505 nm long-pass filtration. At the full imaging frame
rate of 12 fps, the individual non-contiguous fibre spot images
were recorded in real-time and reconstructed as microendoscopic real-time fluorescence maps with ten separate
readings mapped across the occlusal extent of each lesion. For
each field of view (600 mm), the supplied software calculated
the mean numerical fluorescence intensity (arbitrary units).
As there was no contrast in a fully white (i.e. saturated) image,
and no data in a fully black field (sound dentine), the

numerical measure of greyscale represented the degree of

AF saturation of the image. The confocal fibre was peroxidebleached (standardised manufacturer protocol) between every
reading to eliminate fluorescent debris transfer between
measurement sites and between readings from a site. A
subsequent reading was only taken when no fluorescence was
recorded from the probe tip in air, representing a zerocalibration. Readings taken from the exposed sound dentine
acted as internal sample controls. A pilot study confirmed that
contact imaging AF measurements from both sound and
carious dentine samples showed no discernable AF data
variation with darkness to bright daylight ambient conditions.
Ten post-excavation CFOME readings were finally mapped
from the remaining dentine cavity surface following the
protocol outlined above.

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journal of dentistry 38 (2010) 480489

Table 2 The codes used to analyse the mode of failure

and loci of failure on the external surfaces of the stick
samples having undergone microtensile testing.
Code
1
2
3
4
5

Failure mode/locus
Cohesivein dentine
Adhesivebetween dentine/adhesive layer
Cohesivewithin the adhesive
layer
Adhesivebetween adhesive
layer/composite
Cohesivewithin composite

The proportion of each surface to undergo varying modes of failure

was also considered. The coding relates to Fig. 8.

2.4.

Microscope, Madison WI, USA). Samples were illuminated

with a mercury arc lamp and examined using a 20/0.80 NA oil
immersion objective lens in conjunction with a 10 eyepiece
(Olympus, Japan). The failure mode on one external surface of
each beam was determined visually and recorded (see
Table 2) and the sample rotated until all four sides had been
analysed.

2.5.

Statistics

The microtensile bond strength data was statistically analysed

using KaplanMeier survival analysis with Sidaks adjustment
for multiple comparisons. Significance was set at p < 0.01.

3.

Results

3.1.

SEM evaluation

Cavity restoration and microtensile testing

After caries excavation, the 21 samples in each group were

restored either with Adper Scotchbond 1XT/Filtek supreme
resin composite or Filtek Silorane adhesive/Silorane composite,
as per manufacturers instruction. After hydrated four-week
storage, the teeth were first sectioned through the restoration in
a mesio-distal longitudinal plane using a low speed watercooled diamond saw (Labcut, Agar Scientific, Stansted, UK). A
perpendicular section to the adhesivetooth interface followed
to obtain beams (0.9 mm  0.9 mm wide; 57 mm long), each
consisting of composite, adhesive and dentine. Twenty-five
beams were produced from each of the six excavation subgroups. These were fixed with cyanoacrylate glue (Loctite1,
Henkel, Hatfield, UK) to two surfaces on a linear actuatordriven, offset micro-tensile testing device (SMAC, Horsham,
UK), and stressed at a crosshead speed of 1 mm/min until
failure. The micro-tensile bond strength (mTBS) was expressed
in MPa, as derived from dividing the imposed force (N) at the
time of fracture by the bond area (mm2).
In order to evaluate the failure mode of the beam
specimens after fracture, each sample was reassembled,
fixed flat on a glass slide using PlasticineTM and placed on the
stage of a confocal microscope (Noran Tandem Scanning

Representative micrographs for the hand excavation samples

are shown in Fig. 3, CarisolvTM gel excavation, Fig. 4 and SFC-V
(Biosolv), Fig. 5. Low magnification SEMs showed flaky, rough
surfaces with all excavation modalities, but subjectively worse
in the hand excavation group. At higher magnification, a
consistent smear layer was detected in the hand excavation
group causing plugs to form within the tubular orifices
(Fig. 3b). Both chemo-mechanical techniques produced a
reduced and more inconsistent smear layer with large areas
of open tubular orifices in the CarisolvTM group (Fig. 4) and a
greater mixture of open and closed tubules in the SFC-V
(Biosolv) group (Fig. 5).

3.2.

CFOME AF measurements

Table 3 outlines the AF numerical data from the samples from

each experimental group, pre- and post-excavation. Consistently elevated AF data was produced from the original cariesinfected dentine pre-excavation across all experimental
groups. Significant reduction in the AF data post-excavation
was apparent in all experimental groups indicating the

Fig. 3 Scanning electron micrographs of epoxy resin replicas of the dentine surface remaining after conventional hand
excavation. (a) 1.0k magnification showing smearing of the dentine surface and tubule occlusion. (b) 5.0k magnification
showing a structureless smear film and plugs within the tubule orifices.

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journal of dentistry 38 (2010) 480489

Fig. 4 Scanning electron micrographs of epoxy resin replicas of the dentine surface remaining after CarisolvTM gel
excavation. (a) 800T magnification showing a dentine surface with open tubule orifices. (b) 2.0k magnification showing a
lack of smear layer and opened tubules.

Fig. 5 Scanning electron micrographs of epoxy resin replicas of the dentine surface remaining after SFC-V (Biosolv) gel
excavation. (a) 1.0k magnification showing an area of smear plug-filled tubular orifices. (b) 1.0k magnification showing an
area of opened tubular orifices.

removal of infected dentine. Hand-excavated samples showed

the greatest reduction in AF (to a mean value of 69) indicating
potential over-preparation into histologically sound dentine.
Out of the two chemo-mechanical groups tested, CarisolvTM

gel excavation tended to remove a more consistent amount of

dentine (smaller standard deviation; mean AF value 130) and
SFC-V tended to leave more residual carious dentine behind
(mean AF value 269).

Table 3 Mean AF data (arbitrary units) plus standard deviations (SD) for each experimental group, before and after caries
excavation, measured using CFOME.
Scotchbond 1XT/Filtek Supreme (N = 21)

AF pre-excavation

SD

AF post-excavation

Hand (N = 7)
CarisolvTM (N = 7)
SFC-V Biosolv (N = 7)

1897.50
2241.86
2064.00

682.38
533.75
592.42

61.76
126.11
264.71

30.82
37.53
79.30

Filtek Silorane bond/composite (N = 21)

Hand (N = 7)
CarisolvTM (N = 7)
SFC-V Biosolv (N = 7)

1704.00
2317.86
2200.00

620.18
594.57
486.19

60.79
134.49
274.00

30.53
38.43
88.42

SD

Ten readings per tooth both pre- and post-excavation were analysed. CFOME was calibrated against ambient lighting conditions and internal
sound dentine controls (0 reading indicates no fluorescent signal).

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journal of dentistry 38 (2010) 480489

Fig. 6 Microtensile bond strength data for the Scothbond

1XT/Filtek Supreme experimental group (H, hand
excavation; C, CarisolvTM; and B, SFC-V Biosolv). Mean
data for each sub-group calculated from the 50% survival
rate. Sidaks multiple comparison analysis indicated a
significant difference between hand excavation and
CarisolvTM groups.

3.3.

Microtensile bond strengths

In the etch-and-rinse group the mean value of the microtensile bond strengths obtained after four weeks hydrated
storage was 27 MPa (SD 3.9) for hand excavation, 22 MPa (SD
5.1) for CarisolvTM and 26 MPa (SD 4.4) for SFC-V. This data was
analysed using KaplanMeier survival analysis (Fig. 6) with

Fig. 7 Microtensile bond strength data for the Filtek

Silorane bond/composite experimental group (H, hand
excavation; C, CarisolvTM; and B, SFC-V Biosolv). Mean
data for each sub-group calculated from the 50% survival
rate. Sidaks multiple comparison analysis indicated a
significant difference between hand excavation and each
of the two chemo-mechanical excavation groups.

Sidaks adjustment for multiple comparisons which indicated

that there was a significant global difference between the
survival curves ( p = 0.01). Sidaks multiple comparison indicated that there was no significant difference between hand
excavation and SFC-V subgroups or between CarisolvTM and
SFC-V. There was however, a significant statistical difference
in the microtensile bond strengths between the hand
excavation and CarisolvTM groups.
In the case of the self-etch group, the mean value of the
bond strengths obtained was 22 MPa (SD 3.3) for hand
excavation, 27 MPa (SD 6.1) for CarisolvTM and 25 MPa (SD
4.7) for SFC-V. Again, the bond test data was analysed using
the above-mentioned statistics (Fig. 7), where Sidaks multiple
comparison indicated that there was no significant difference
between the CarisolvTM and SFC-V subgroups. There was a
significant difference between hand excavation and CarisolvTM, and between hand excavation and SFC-V.

3.4.

Analysis of failure modes

The locus and type of failure was described and coded in

Table 2 and the distribution of failure, examined from the four
external surfaces of each matchstick sample, have been
graphically illustrated in Fig. 8. In the etch-and-rinse samples,
an even distribution of failure types 2, 3 and 5 were noted with
a small number of cohesive dentine failures across the subgroups (type 1). In the self-etch Silorane samples, adhesive
failures between the bond and composite predominated (type
4) with further even distributions of cohesive failures within
the bond layer and composite, respectively. There were fewer
adhesive failures between dentine and the bond layer (type 2)
in the self-etch Silorane samples than the total-etch Scotchbond samples, independent of the excavation techniques
used.

Fig. 8 Graph showing the % distribution of the five

different failure modes (Table 2) in each of the
experimental groups (SB, Scotchbond/Supreme samples;
SA, Silorane bond/composite samples; H, hand
excavation, C, CarisolvTM, B, SFC-V Biosolv). From the
data it can be seen that the predominant failure in the selfetched Silorane samples was type 4 (between the adhesive
layer and the composite) whereas for the Scotchbond
total-etch samples, there were even proportions of
predominantly type 2, 3 and 5 failures.

journal of dentistry 38 (2010) 480489

4.

Discussion

This study aimed to investigate a number of null hypotheses

simultaneously within the same natural carious tooth
samples, so enabling clinical relevance to emerge from an
in vitro study. A single trained operator was used in order to
minimise inter-operator variability in this study, but the
potential for clinical variation in the use of these technologies
might be worthy of future investigation.
There are no differences in the amount and quality of
carious dentine excavated by three different clinical hand
excavation techniques (CarisolvTM gel, SFC-V and hand
excavation).
Two chemo-mechanical agents were compared against
each other and conventional hand excavation in this study.
Caries removal was guided by the self-limiting nature of the
technique and/or the hardness of the dentine remaining.
Using novel CFOME technology to measure the AF level of
initial and residual caries, enabled an objective, in situ
assessment of the type of dentine remaining and the quality
of that tissue excavated. A previous study has calibrated the
fluorescent saturation intensity levels for infected, affected
and sound dentine against its microhardness.14 The data
presented here indicated that hand excavation tended
towards over-preparing the dentine, leaving histologically
sound cavity walls (AF < 100; mean reading 69). Both chemomechanical systems, arguably more self-limiting due to the
collagenolytic action of the sodium hypochlorite in CarisolvTM
gel or pepsin in SFC-V coupled to a more controlled abrasive
mechanical action of the mace-tip metal instrument, tended
to leave some residual caries-affected dentine. CarisolvTM gel
left dentine with a mean AF value of 130 whereas SFC-V
resulted in dentine with a mean AF value of 269, implying
clinical under-preparation in certain areas. These findings, in
terms of clinical operative minimally invasive dentistry, are
acceptable and arguably more desirable if ultimately, a sealed
adhesive restoration can be placed.
The scanning electron microscopy analysis of the excavated dentine surfaces using resin replicas is a tried and tested
method, permitting accurate subjective analysis of surface
topographical features.17 The findings from this study indicated that the chemical agents in CarisolvTM gel had the ability
to alter significantly the smear layer created by the mechanical
action of the abrading instrumentation used. SFC-V Biosolv
subjectively did not appear to be as efficient in smear layer
removal. This might be due to the rapid neutralisation of the
acidic pH on the dentine surface, so reducing the efficacy of
the pepsin action on the organic component of the smear
layer.
These findings led to the conclusion that each caries
removal technique left dentine surfaces that were histologically different from one another, thus rejecting the first
proposed null hypothesis.
Using three different caries excavation techniques (CarisolvTM gel, SFC-V and hand excavation) has no effect on
adhesive bond strengths to residual carious dentine, when
comparing total-etch and self-etching dentine bonding systems.
Analysis of Figs. 6 and 7 revealed that using different caries
excavation techniques did have an effect on the microtensile

487

bond strength (mTBS) of adhesives to dentine. This finding was

in agreement with Sonoda et al.26 and Tosun et al.30 but
conflicted with Cehreli et al.23 Moreover, the two types of
adhesives used in this study reacted differently with the
varying histological types of dentine left after caries removal,
in agreement with Tosun et al.30 and Koyuturk et al.22 but in
conflict with the findings of Nakornchai et al.21
The CFOME AF measurements indicated that hand excavation tended towards over-preparation with more histologically sound dentine at the cavity walls. SEM examination
showed that hand excavation produced smearing and smear
plugs in the tubular orifices. Interestingly, Scotchbond 1XT
(two-step, etch-and-rinse adhesive) produced the highest
mTBS to this dentine compared to mTBS to residual carious
dentine remaining after the chemo-mechanical techniques.
However, the Filtek Silorane bond (two-step, self-etching
primer adhesive) samples exhibited the lowest mTBS to the
sound dentine. Although the dentine that is left after caries
removal using hand excavation has similar hardness to that of
normal sound dentine, there are ultra-structural differences.
It is known that as caries progresses, translucent dentine
(sclerotic dentine) is deposited within the tubules at the
advancing front of the lesion, that can lead to their complete
obliteration. This fact, in conjunction with the formation of a
smear layer that has a higher organic content, due to the
increased bacterial load, may interfere with ability of the
relatively mild self-etching Silorane adhesive to penetrate this
smear layer and demineralise the underlying dentine thus
leading to a reduced mTBS compared to that of the etch-andrinse Scotchbond 1XT adhesive. Studies that used caries
excavation techniques that tended to over-prepare cavities
and form a thick smear layer (for example, round steel burs,
lasers and abrasive silicon paper sample preparation techniques) all reached similar observations, that the etch-and-rinse
adhesives demonstrated stronger bond strengths to cariesaffected dentine than the self-etch adhesives20,29,31. It was
demonstrated that the use of conventional hand excavation
appears to weaken the bond strength of self-etch adhesives to
the remaining dentine and they attributed this finding to the
presence of an infected smear layer.26
CFOME indicated that CarisolvTM gel excavation was more
selective than hand excavation leaving residual caries-affected dentine which is partially demineralised; the intertubular
dentine exhibits a high degree of porosity and some of the
dentinal tubules are filled by more acid-resistant mineral
crystals (whitlockite).32 SEM also indicated that CarisolvTM gel
produced a roughened surface with minimal smear layer
coverage of the dentine surface leaving mainly open tubular
orifices. The self-etching Silorane adhesive established a
stronger bond to this dentine than the etch-and-rinse
Scotchbond 1XT adhesive. It was found that self-etch
adhesives penetrate deeper and form a thicker and smoother
hybrid layer when CarisolvTM gel was used to remove caries.23
The authors assumed that the removal of the smear layer by
the action of CarisolvTM gel allowed the self-etch adhesive to
penetrate deeper than when it was applied to a smear layercovered dentine. Sonoda et al. also confirmed that self-etch
adhesives exhibited improved bond strengths to dentine
remaining after CarisolvTM excavation.26 In the case of etchand-rinse Scotchbond 1XT adhesive, it was assumed that the

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journal of dentistry 38 (2010) 480489

removal of the smear layer by the action of CarisolvTM gel

permitted the phosphoric acid etch to demineralise dentine to
a deeper depth so exposing a thicker collagen layer. This
thicker collagen layer may have prevented full penetration of
the adhesive leaving an inner layer of collagen poorly
embedded with resin. In addition, the presence of acidresistant crystals in the dentinal tubules may have interfered
with resin tag formation.33 All of these factors may be
attributable to the lower bond strength values obtained when
bonding Scotchbond 1XT adhesive to dentine remaining after
caries removal using CarisolvTM gel.
Using enzymes to enhance hand excavation is a relatively
new concept in caries research.4,15 SFC-V Biosolv is an
experimental gel that unlike CarisolvTM does not contain
NaOCl but instead it contains pepsin as its active ingredient.
Furthermore, CarisolvTM is highly alkaline (pH 12) whilst SFCV is acidic (pH 3) in nature. The results of this study showed
that the more acidic SFC-V Biosolv chemo-mechanical
excavation left behind a softer and rough dentine surface
topography with varying levels of smear layer, different to that
observed with the CarisolvTM samples. Both these factors
contributed to the mTBS values indicating that the type of
dentine remaining after SFC-V Biosolv excavation was
compatible with both etch-and-rinse Scotchbond 1XT and
self-etching primer Silorane adhesives.
This investigation did not endeavour to assess the longer
term durability of adhesive bonds to carious dentine and there
is evidence that these interfaces may undergo more rapid
long-term hydrolysis, phase separation of the hydrophilic and
hydrophobic components and/or breakdown due to the action
of dentine metallo-matrix proteinases (MMPs). This aspect of
adhesive bonding to dentine requires further investigation. It
is essential that, in a clinical situation, optimal enamel
margins are maintained to obtain the best peripheral seal
achievable. However, in this study, the results of microtensile
bond strength testing meant that this null hypothesis was also
rejected.
Using three different caries excavation techniques (CarisolvTM gel, SFC-V and hand excavation) has no effect on the
failure mode and loci of failure when bonding to the residual
carious dentine, comparing total-etch and self-etching dentine bonding systems.
The adhesiverestorative interface is comprised of five
aspects from the dentine side across to the composite,
through the adhesive (bond) layersee Table 2. This study
used confocal microscopy to analyse the external surfaces of
the stick samples, permitting a more detailed evaluation of
the failure type and loci from mTBS studies. Most of these tend
to analyse the two plane-ended fracture surfaces end-on,
often with SEM. The interpretation of the surface topography
and structure can be difficult and open to interpretation.
Using the present technology, a more detailed picture of the
variability in the fracture mode and position was formed. It
was apparent from the data that samples in all groups
suffered similar proportions of cohesive failure in the
composite aspect of the restorative interface. The self-etch
Silorane bond samples did not suffer any cohesive failures in
dentine, even within the chemo-mechanical caries excavation groups which left residual, softer caries-affected dentine.
This was possibly due to the deeper infiltration of the self-

etching primer and adhesive into the affected dentine with a

reduced smear layer so potentially reinforcing the tissue
against cohesive failure as well as the fact that Filtek Silorane,
due to its ring-opening siloxaneoxirane chemistry, exhibits
very low polymerisation shrinkage (0.9%). This would generate less shrinkage stress at the adhesive interface, so
reducing the forces tending to pull the structurally weaker
affected dentine apart. The Silorane group did suffer from a
proportion of type 4 failures (between adhesive and composite) potentially indicating a less robust interface in some
samples that those created by the etch-and-rinse DBA and
resin composite combination and this finding might require
further investigation. From both adhesive groups, etch-andrinse and self-etch, it was apparent that broadly similar
proportions of failure type and locations were observed
across the three excavation sub-groups.
Therefore, again, this null hypothesis was rejected from the
presented data.

5.

Conclusions

The three caries hand-excavation techniques used in this

study retained varying histological qualities of sound
through to affected dentine at the cavity walls postexcavation (hand excavation > CarisolvTM gel > SFC-V Biosolv, respectively) and the CFOME instrument was useful in
analysing this tissue via its AF signal, in situ objectively.
This fibre-optic technology may be developed for future
clinical use. The microtensile bond strengths and failure
modes of the two types of adhesive (etch-and-rinse vs. selfetch) showed variations in their ability to adhere to the
differing dentine structure and a range of failure types
throughout the adhesive interface. The low-shrink Silorane
adhesive/composite system appeared to exert less stress on
the dentineadhesive interface.

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