Journal of Dental Research

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In vivo Degradation of Resin-Dentin Bonds in Humans Over 1 to 3 Years

M. Hashimoto, H. Ohno, M. Kaga, K. Endo, H. Sano and H. Oguchi
J DENT RES 2000 79: 1385
DOI: 10.1177/00220345000790060601

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M. Hashimoto'*, H. Ohno2, M. Kaga',
K. Endo2, H. Sano3, and H. Oguchi'
' Department of Pediatric Dentistry, School of Dentistry,
Hokkaido University, Kita 13, Nishi 7, Kita-ku, Sapporo 060-
8586, Hokkaido, Japan; 2Department of Dental Materials Science,
School of Dentistry, Health Sciences University of Hokkaido,
Ishikari-Tobetsu 061-0293, Hokkaido, Japan; and 3Department of
Operative Dentistry, School of Dentistry, Hokkaido University;
*corresponding author, masanori-h(.mue.biglobe.ne.jp
J Dent Res 79(6): 1385- 1391, 2000
ABSTRACT
The longevity of resin restorations is currently an
area of great interest in adhesive dentistry. However,
no work has been conducted to investigate the
durability of resin-dentin bond structures using
human substrate in vivo. The purpose of this study
was to investigate the degradation of the resin-
dentin bond structures aged in an oral environment
for 1, 2, or 3 years. Cavities were prepared in
primary molars, and an adhesive resin system
(Scotchbond Multi-Purpose) was applied to the
cavity. After 1 to 3 years, following the eruption of
the succedaneous permanent teeth, the resin-restored
teeth were extracted. Immediately after extraction,
those teeth were sectioned perpendicular to the
adhesive interface and trimmed to produce an
hourglass-shaped specimen. Then, a micro-tensile
test was performed at a crosshead speed of 1.0
mm/min. The mean bond strengths were statistically
compared with one-way ANOVA and Fisher's
PLSD test (p < 0.05). Further, all fractured surfaces
were observed by SEM, and the area fraction of
failure mode was calculated by means of a digital
analyzer on SEM photomicrographs. There were
significant differences in tensile-bond strength
among all 3 groups (p < 0.05), with mean values
ranging from 28.3 ± 11.3 MPa (control), to 15.2 i
4.4 MPa (1 to 2 years), to 9.1 ± 5.1 MPa (2 to 3
years). Moreover, under fractographic analysis, the
proportion of demineralized dentin at the fractured
surface in specimens aged in an oral environment
was greater than that in control specimens.
Furthermore, degradation of resin composite and the
depletion of collagen fibrils was observed among
the specimens aged in an oral environment. Analysis
of the results of this study indicated that the
degradation of resin-dentin bond structures occurs
after aging in the oral cavity.
KEY WORDS: degradation, dentin bond durability,
fractography, micro-tensile bond test.
Received July 12, 1999; Last revision November 15, 1999;
Accepted November 30, 1999
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In vivo Degradation
of Resin-Dentin Bonds
in Humans Over 1 to 3 Years
INTRODUCTION
N umerous studies have been conducted to evaluate the integrity of resin-
dentin bond structures. However, most of the experiments in those studies
were performed over short periods, such as 24 hours. Several investigations
have recently attempted to evaluate the durability of resin-dentin bonds during
long-term storage in water (Kiyomura, 1987; Gwinnett and Yu, 1995; Burrow
et a!., 1996). Those studies demonstrated a reduction in bond strength during
long-term immersion in water. Gwinnett and Yu (1995) reported that the bond
strength of All-Bond 2 and Amalgambond to dentin decreased after 6 months'
water immersion. Moreover, Burrow et al. (1996) reported a decrease in bond
strength of Photo Bond to dentin during 3 years in water.
Incomplete resin impregnation in the collagen network leaves an exposed
demineralized dentin zone at the base of the hybrid layer (Nakabayashi and
Takarada, 1992; Sano et al., 1994, 1995; Titley et al., 1994; Nor et al., 1996).
Hence, it has been speculated that the region of the exposed collagen fibrils is
susceptible to hydrolytic degradation over a long period, leading to a
reduction in bond strength (Kiyomura, 1987; Nakabayashi and Takarada,
1992; Burrow et al., 1996).
Sano et al. (1999) investigated the resin-dentin bonds of Liner Bond II
after 1 year in the oral cavities of monkeys, using a micro-tensile test.
Although analysis of the results revealed no reduction in bond strength,
morphological changes in the resin composite and adhesive resin were
observed at the fractured surface over time. However, no report is available
on the bond strength and morphological changes in the bond structures of
human dentin substrates aged in an oral environment for long periods.
Therefore, it was the aim of this study to use micro-tensile testing to clarify
whether bond strength is reduced with time in the oral cavity. Moreover,
fractographic analysis was used to characterize morphological changes in the
resin-dentin bond structures of human substrates aged in an oral environment
for 1 to 3 years.
MATERIALS & METHODS
Resin Composite Filling
The subjects were outpatients who attended the Department of Pediatric
Dentistry of Hokkaido University for treatment of caries. Informed consent was
obtained from all subjects under a protocol approved by the appropriate
institutional review board. The primary molars, which exhibited dental caries
involving the dentin, were anesthetized with local anesthesia, and then the
cavities were prepared by means of a diamond point in a high-speed handpiece
with copious water spray under rubber-dam isolation. The entire carious region
was carefully removed, with a caries-detecting dye solution (Caries Detector,
Kuraray Co., Osaka, Japan) as a guide. The class II cavities were located on the
mesial and distal aspects of the occlusal surfaces, including a proximal surface of
approximately 4 to 5 mm (mesial to distal) x 2 to 3 mm (buccal to lingual) x 2
mm (depth). A commercially available dentin adhesive system (Scotchbond
1385
 1386 Hashimoto et a/. J Dent Res 79(6) 2000
Multi-Purposc, 3M Dental Products, St. Paul, MN, USA) was used form a gentle curve along the bonded interface fiom both sidcs
in this study. The prcpared cavity was treated with an acid until 1.0 mm2 of bonded surface remainied (Fig. ). These
conditioner (Etchant: 10% maleic acid and polyvinyl alcohol specimens were then attached to a testing apparatus with a
thickener) for 15 sec, then thoroughly washed in a water spray. cyanoacrylate adhesive (Model Rcpair 11 Bluc, Sankin Industry
Excess water was removed with a short blast of air, leaving the Co., Ltd., Tokyo, Japan), and a tensile load was applied by a table-
surface visibly moist (Swift and Triolo, 1992; Van Meerbeek et al., top material tester (EZ Test, Shimadzu Co., Kyoto, Japan) at a
1998). A priming agent (Primer: an aqueous solution of HEMA crosshead speed of 1.0 mm/mill.
and polyalkenoic acid co-polymer) was then applied for 10 sec and To invcstigatc differenccs in tensile bond strength and
dried with a gentle stream of air. A thin layer of bonding resin morphological appearancc of the fractured surface between bond
(Adhesive: Bis-GMA and HEMA) was applicd and light-cured for st-uctures aged for short and long periods, wc also prcpared control
10 sec with a light-curing unit (Visilux 2, 3M Dental Products, St. specimens in this study. Thirteen non-cai ious primary molars werc
Paul, MN, USA). After the bonding resin was applied, the cavities extracted for orthodontic purposes with the iiformcd conscit of
were filled with 2 layers of a rcsin composite (Z I00: Bis-GMA and the donors. The class 11 cavities were prepared in the teeth by
filler) and cured by irradiation with light for 60 sec for each layer. means of a diamond point in a high-speed handpiccc with copious
All of the above procedures were performed by one clinician. water spray. The form of the cavities was prepared in the same
manner as that of oral cavity specimens. A dentini-bonided resin
Micro-tensile Bond Test system was then applied in the cavity as previously described.
After I to 3 yrs, as the permanent teeth erupted, the resin-filled After the resin-restored specimens had been stored in distilled
teeth were extracted with the informed consent of the donors. The water at 37°C for 24 hrs, 2 hourglass-shapcd sections wcre
extracted teeth were rinsed and stored in distilled water at 4°C for prepared from each tooth. A micro-teinsile bond test was conducted
a period not exceeding 2 wks. Those teeth that were free of caries immediately at a crosshead speed of 1..0 mm/mill.
and marginal discoloration were selected by means of a
stereoscopic microscope (SMZ-IOA, Nikon Co., Tokyo, Japan). Fractographic Analysis
The distribution of the teeth is shown in the Table. The resin-filled After micro-tensile bond testing had been completed, all fractlied
teeth were scctioned perpendicular to the adhesive interface by surfaces were sputter-coated with gold (lon sputter E-1030. I litachi
means of a diamond saw (Isomet, Buehler Ltd., Lake Bluff, IL, Ltd., Tokyo, Japan) and observed with a ficld-cmission scanninig
USA) with a water coolant. One or two resin-dentin bonded electron microscope (S-4000, Hitachi Ltd., Tokyo, Japan). To
sections were obtained per tooth. The teeth with flat, regular cavity calculate the bond strength in MPa, wc tised SEM
floors were used as test specimens. These slices were carefully photomicrographs to measure the adhesive areas on the dentin side
trimmed and shaped with a superfine diamond point (SF 1104R, of the fractured surface. The bond strengthis obtained were
Shofu Co., Ltd., Kyoto, Japan) to produce an hourglass shape to analyzed by one-way ANOVA and Fisher's PLSD test, with a p-
value of less than 0.05 regarded as significanlt. Fractographic
Table. Distribution of Teeth
Specimen Site Period in Oral Cavity Resin composite filling
in a cavity
I L.R.S. 1 yr 0 mo
2 L.R.S. 1 yr 1 mo
3 L.R.S. 1 yr 1 mo
4 L.L.F. 1 yr 2 mo
5 U L.S. 1 yr 3 mo
6 L.L.S. 1 yr 4 mo
7 L.L.S. 1 yr 5 mo i After 1 to 3 years
8 U.L.F. 1 yr 8 mo Sectioned perpendicular to
9 U.R.F. 1 yr 9 mo the adhesive interface using
10 L.R.S. Iyr 10 mo a diamond saw
11 LR.F. 1yrli mo
12 L.R.S. 2yr0mo
13 U.L.S. 2yrl mo
14 L.R.S. 2yr2mo
15 U.R.S. 2yr2mo
16 L.R.F. 2yr3mo
17 U.L.F. 2yr5mo Trimme( I to produce
18 U.L.S. 2yr7mo an hourglass shape using
19 L.L.S. a superfine diamond point
2yr9mo
20 L.L.S. 2 yr 9 mo Adhesive area 1.0 mm2
21 L.R.F. 2 yr 11 mo
22 U.R.S. 3 yr 0 mo a =Y
C II -wor 11 In r -h.1 .11 Rirh F) Pr iI.-r 7 fir_t
I-, m l rS.,
t' -'
-
-1 ... I ... -- ,

Primary -s'ec`o'n.[molar.'
' -
Figure 1. Specimen preparation for micro-tensile bond test.
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J Dent Res 79(6) 2000 In vivo Degradation of Resin-Dentin Bonds in Humans 1 387

analysis was performed by observation of the fractured surface of

the dentin side by SEM.
To clarify the weakest zone within the resin-dentin bond
structures, we assigned the failure modes to one of the following
groups: (I) failure in the bonding rcsin or rcsin composite; (11) in
the hybrid layer; (111) in the demineralized dentin zone; and (IV) in
the dentin. Thc area fraction of each failure mode on the dentin
side was examined with a digital analyzer (Digitizer KD403OB;
GRAPHTEC, Tokyo, Japan) on SEM photomicrographs.

RESULTS
The bonded surface areas at the dentin side of the fractured
surface, calculated by means of SEM photomicrographs (90x),
were 0.94 ± 0.17 mm2 (48 specimens). There were significant
differences in tensile-bond strength among all 3 groups (p <
0.05), with mean values ranging from 28.3 ± 11.3 MPa (24 hrs),
to 15.2 ± 4.4 MPa (I to 2 yrs), to 9.1 i 5.1 MPa (2 to 3 yrs).
Fig. 2a shows the total fractured surface on the dentin side
of a restoration with a bond strength of 11.3 MPa aged in an
oral environment for 1 yr 1 mo. The sections marked (b), (c),
(d), (e), and (f) in the Fig. are shown as SEM photomicrographs
at higher magnifications in Fig. 2b, 2c, 2d, 2e, and 2f,
respectively. Typical cohesive failure of the dentin can be seen
in Fig. 2b. Fig. 2c shows evidence of resin impregnation into
the collagen fibrils. In Fig. 2d, open spaces between collagen
fibrils can be seen without any evidence of resin impregnation
or of peritubular dentin matrix. Both the orifices of dentinal
tubules and those of lateral branches can be seen in Fig. 2e. In
Fig. 2f, several filler particles were detached from the resin
matrix, and a crack was formed at the filler-matrix interface.
The area fractions of the failure mode, as shown in Fig. 2g, are:
8.2% in the resin composite or bonding resin, 20.7% in the
hybrid layer, 37.0% in the dentin, and 34.1% in the
demineralized dentin.
The area fraction of the various failure modes for each time
period is shown in Fig. 3a (lower). Fig. 3b shows the relationship
between the bond strength and the area fraction of the failure
mode, obtained from the control specimens (upper) and from
those aged in an oral environment for I to 3 yrs (lower).
The area of resin composite at the fractured surface of the
control specimen is shown in Fig. 4b.

DISCUSSION
The appearance of mineralized peritubular dentin indicates
that this subsurface region was not affected by acid treatment
(Fig. 2b). In Fig. 2c, the scratch marks (white arrows)
observable on the fractured surface and the impregnation of Figure 2a. Fractured surface on the dentin side of a specimen with a
collagen fibrils with adhesive resin indicated that the fracture bond strength of 11 .3 MPa aged in an oral environment for 1 yr 1 mo.
occurred at the top of the hybrid layer. In Fig. 2d, the presence
of exposed collagen with open spaces between the fibrils and
without any evidence of resin impregnation suggested that the degradation, leading to a reduction in bond strength during
fracture occurred in the demineralized dentin which existed long-term storage in water (Kiyomura, 1987; Nakabayashi and
beneath the hybrid layer. The fractured surface of the Takarada, 1992; Burrow et al., 1996).
demineralized dentin zone in the control specimens was In Fig. 2e, the lateral branches of dentinal tubules can be
similar to that in Fig. 2d, indicating that this zone was created observed in the intertubular dentin of an experimental tooth
at the time of resin application (Nakabayashi and Takarada, functioning in the mouth for I yr I mo. Fig. 4a shows a dentin
1992; Sano et al., 1994, 1995; Titley et al., 1994; Nor et al., surface in a control tooth treated with 100% sodium
1996). From a clinical standpoint, it has been predicted that hypochlorite for 10 min after acid conditioning with 10%
exposed collagen fibrils are susceptible to hydrolytic maleic acid for 15 sec. In this SEM microphotograph (Fig. 4a),
Downloaded from jdr.sagepub.com at TEXAS SOUTHERN UNIVERSITY on October 28, 2014 For personal use only. No other uses without permission.
 1388 Hashimoto et al.
the diameter of the dentinal tubules is approximately 2 to 3 Itm
and that of the lateral branches is approximately I to 2 ,m,
indicating that the lateral branches increased in diameter
proportionally more thani did the dentinal tubules. The
peritubular matrix of the dentinal tubules was rich in inorganic
matter as compared with that of the lateral branches. Hence,
the organic matrix surrounding the lateral branches was readily
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J Dent Res 79(6) 2000
Figures 2b-2f. Higher magnifications of the areas of the fractured
surface marked (b)-(fl on Fig. 2a.
removed by the sodium hypochlorite. A similar
micromorphologic appearance, except for the presence of resin
tags, was observed at the fractured surfaces of several
specimens aged in an oral environment, as shown in Fig. 2e. It
is speculated that the mineral matrix seen in Fig. 2e was left as
a result of the depletion of the collagen fibrils. Microstructural
evidence suggests that the collagen and gelatin of the exposed
collagen network were digested by proteolytic enzymes
(Okada and Ikada, 1992), which were released from
leukocytes, salivary glands, and bacteria in plaque (Uitto and
Raeste, 1978; Kowashi et al., 1979). Hence, the hypothesis
that the exposed collagen fibrils were susceptible to hydrolytic
degradation (Kiyomura, 1987; Nakabayashi and Takarada,
1992; Burrow et al., 1996) was confirmed.
Detached filler particles and the formation of a gap at the
filler-matrix interface can be seen in the magnified section of
resin composite (Fig. 2f) from a specimen aged in an oral
environment. No such particles were present at the fractured
surface of the control specimen shown in Fig. 4b. Ferracane et
al. (1995) found that the fracture toughness of a commercially
available resin composite (ZIOO as used in this study) was
reduced by approximately 15% after 10 days and by 45% after
J Dent Res 79(6) 2000 In vivo Degradation of Resin-Dentin Bonds in Humans 1 389
40 days of storage in 37°C water. The reduction in mechanical
properties of the resin composite is related to water sorption
within the main chains and cross-links of the resin matrix,
which may induce the expansion of the cross-linked polymer
network (Soderholm, 1984; Drummond et al., 1998). The
uptake of water induces stress between the softer matrix and
the stiff filler particles, leading to filler-matrix interfacial
failure and the formation of cracks in the matrix (Soderholm et
al., 1984). In addition, the chemisorbed silane layers on the H
inorganic filler particles are susceptible to hydrolytic attack by
the absorbed water (Craig and Dootz, 1996). Moreover, it has
been demonstrated that food-simulating liquids (McKinney
and Wu, 1985), organic acids (Asmussen, 1984), enzyme
simulators (Bean et a!., 1994), and solvents (Asmussen, 1984;
Ferracane and Berge, 1995) accelerated the degradation of the
resin composite. Furthermore, physical elements such as
masticatory and occlusal stresses may promote the degradation DD
of the composite materials in an oral environment. Therefore,
the reduction in mechanical properties of the resin composite
in an oral environment is thought to be greater than that in in
vitro conditions.
From SEM observations of the fractured surface on the
dentin side, the area fractions of failure modes for all R
specimens were calculated in the same manner as that
illustrated in Fig. 2g.
Fig. 3a shows that the bond strengths of the control
specimens were significantly higher than those of the other
groups (p < 0.05). In this study, teeth with carious regions
were used for the specimens to be aged in an oral environment.
The normal and the inner parts of caries-affected dentin, where
not stained by the caries-detecting dye, were both present on * bonding resin or resin composite (R), M dentin (D),
the prepared dentin surface after removal of the outer part of 17| hybrid layer (H), D1 demineralized dentin (DD)
the dye-stained caries-affected dentin. Nakajima et al. (1995)
reported that the bond strengths obtained with the use of Figure 2g. Distribution and area fractions of the failure mode shown in
Scotchbond Multi-Purpose were similar in the normal and the Fig. 2a.
inner regions of the caries-affected dentin. Hence, it was
confirmed that the bond strengths of the specimens aged in an result suggests that resin composite and bondinig resin
oral environment in the present study were not affected by the degraded when aged in an oral environment for a long time
dentin surface conditions, or by the presence of either normal period, and thus bond failure is readily initiated in this zone,
or caries-affected dentin. leading to an increased amount of resin at the fractured
In the specimens aged in an oral environment, the surface. These results coincided with the morphological
proportion of demineralized dentin at the fractured surface appearance of the resin composite, as showin in Fig. 2f.
appeared to be greater than that in the control specimens. The Many in vitro studies have compared the bond strengtlh of
deinincralized dentin zone was found to represent a lesser resin to primary dentin with that to permianent dentini (Fagan ct
proportion of the fractured surface in the control specimens. al., 1986; Salama and Tao, 1991; Bordin-Aykiroyd et a!., 1992).
This indicates that the exposed collagen fibrils were degraded Nor et al. (1996), using Multi-Purpose and All-Bond 2, founld
during aging in an oral environment, and therefore the bond that the hybrid layer was significantly thicker in primary teeth
failure developed at this region over time. Analysis of the than in permanent teeth, resulting in deeper demineralization of
results for the control specimens shown in Fig. 3b indicates the intertubular dentin by acid conditioning. Moreover,
that the area fractions of cohesive failure in the resin and demineralized dentin was more easily created within the bond
dentin were larger in the specimens with higher bond structure of primary dentin than that of permanent dentin.
strengths. There was a clear difference between the specimens Analysis of these findings suggests that the integrity of the
with a bond strength of 10 to 20 MPa and those with a bond bond structures of primary teeth is different from that of
strength greater than 30 MPa. Analysis of the results suggests permanent teeth. However, there has been no evaluation of the
that the higher proportion of the fractured surface was long-term durability of human dentin bonds under in vivo
occupied with the materials of the higher mechanical property conditions. Further in vivo research in humans will be required
such as the resin or the dentin. A comparison of the failure to verify the difference between bond durability of resin to
modes of specimens with a bond strength of 10 to 20 MPa primary and permanent teeth and between bond durability of
shows that the area fraction of resin in the aged specimens was Multi-Purpose and the other adhesive systems.
greater than that in the control specimens. Analysis of this Analysis of the results of this study suggested that
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 1390 Hashimoto et a/. J Dent Res 79(6) 2000
40 Control specimens (24h)

(8) (8) (10)

100
30

toiLi0 20
V. 50

~a
H 10 a.)
10
0
(11):
(I
St-
0 0
24h 1-2y 2-3y period 0-10 10-20 20-30 30 range of bond
strength (MPa)
0 0 0
U'j
0
'-00 4.-:

S
la
a.)
v
CQ
50
50
0
'4

100
(26) (1 1) (1 1)
m bonding resin or resin composite (R), m dentin (D),
LI hybrid layer (H), LI demineralized dentin (DD)
Figure 3a. Relationship between tensile bond strength (upper) and area
fractions of failure modes (lower) on fractured surfaces by period after
bonding; 24 hrs, 1 to 2 yrs, and 2 to 3 yrs. (n) = number of specimens.
100
(9) (13)
Specimens aged in an oral environment (1 to 3y)
m bonding resin or resin composite (R), M dentin (D),
D hybrid layer (H), E] demineralized dentin (DD)
Figure 3b. Relationship between tensile bond strength and area
fractions of failure modes on the fractured surfaces: control specimens
(upperl; specimens aged in an oral environment (lower). (nl = number
of specimens.

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