Eur J Oral Sci 2009; 117: 597–603 ! 2009 The Authors.

Printed in Singapore. All rights reserved Journal compilation ! 2009 Eur J Oral Sci
European Journal of
Oral Sciences

Xin-Hua Gu1, Cai-Yun Mao1, Cong

Does endodontic post space irrigation Liang1, Hui-Ming Wang1, Matthias
Kern2
affect smear layer removal and bonding 1
Department of Stomatology, The First
Affiliated Hospital, College of Medicine,

effectiveness? Zhejiang University, Hangzhou, China;

2
Department of Prosthodontics, Propaedeutics
and Dental Materials, School of Dentistry,
Christian-Albrechts University, Kiel, Germany
Gu X-H, Mao C-Y, Liang C, Wang H-M, Kern M. Does endodontic post space
irrigation affect smear layer removal and bonding effectiveness? Eur J Oral Sci 2009;
117: 597–603. ! 2009 The Authors. Journal compilation ! 2009 Eur J Oral Sci

The effect of different post space irrigants on smear layer removal and dentin bond
strength was evaluated. Sixty-six extracted sound maxillary central incisors were
endodontically treated. After post space preparation, the teeth were assigned to three
groups of 22 teeth each. The teeth of these three groups were irrigated for 1 min with
17% ethylenediaminetetracetic acid (EDTA) (group 1), 5.25% sodium hypochlorite
Professor Dr Hui-Ming Wang, Department of
(NaOCl) (group 2), or 0.9% sodium chloride (NaCl) (group 3). In each group, eight
Stomatology, The First Affiliated Hospital,
specimens were split longitudinally for smear layer evaluation, and the other fourteen College of Medicine, Zhejiang University, #79
specimens were filled with a self-etching adhesive system (Panavia F). Four of 14 Qingchun Road, Hangzhou, Zhejiang Province
specimens of each group were prepared for evaluation of the resin–dentin interdiffu- 310003, China
sion zone (RDIZ) and resin tags, and the other 10 specimens were serially sectioned for
push-out test analysis. Smear layer removal and bond strength were affected by dif- Telefax: +86–571–87236628
E-mail: wangh_m@sina.com;
ferent post space irrigants. EDTA removed the smear layer extremely effectively and, hmwang@zju.edu.cn
as a result, improved the bond strength at each region (apical, middle, and coronal) of
the roots. Resin tag formation and the RDIZ were also affected by different irrigants Key words: bond strength; post space irriga-
and in accordance with bond strength. Therefore, removal of the smear layer use a tion; self-etching adhesive system; smear layer
self-etching luting system plays an important role in bonding effectiveness. Accepted for publication May 2009

Posts and cores are frequently used to restore endodon-
tically treated teeth. Failures of post-supported restora-
tions predominantly result from root fracture and loss of
retention (1). In recent years, fiber posts and resin-based
luting cements have (because of their dentin-matching
mechanical characteristics) been recommended to rebuild
endodontically treated teeth, leading to fewer and
favorable root fractures (2).
Besides reducing the root-fracture risk, adhesive tech-
niques and resin-based luting cements can improve the
post retention through effective and durable bonding
between post and dentin, which is essential for the lon-
gevity of the restorations (3). Previous studies have
suggested that the efficacy of the dentin adhesive mostly
depends upon removal of the smear layer and formation
of the resin–dentin interdiffusion zone (RDIZ) (4, 5).
Moreover, several in vitro studies have demonstrated
that predominant failures of bonding occur at the
cement–dentin interface (6–8). Thus, it is crucial to
improve the bonding effectiveness of the cement–dentin
interface.
The use of self-etching adhesive resin luting systems
for fiber post cementation has shown a recent increase in
popularity. Self-etching adhesive systems incorporate the
smear layer and infiltrate into the partially demineralized
dentin by the use of a primer containing acidic monomer
(9). However, the efficacy of self-etching adhesive to
permeate the smear layer and to impregnate the dentin
still remains a major concern. Some studies have
reported that a thick smear layer reduces the bond
effectiveness of the self-etching adhesive (10, 11), while
others have demonstrated that self-etching adhesive does
not seem to be dependent on the thickness of the smear
layer (12, 13). Yang et al. (14) demonstrated that the
smear layer hybridized by self-etching adhesive was a
weak area in the bonding interface, with the top of the
hybrid layer containing disorganized collagen fibrils that
degrade over time. Therefore, the influence of smear-
layer thickness on the bond strength of self-etching
adhesive systems remains uncertain, and profound
understanding of the role of the smear layer is important
to achieve effective dentin bonding.
Bonding to root-canal dentin might be a challenge
because of the anatomy of the root, handling charac-
teristics of the adhesive systems, and adhesive procedures
(15). Root-canal dentin surfaces were always covered
with a thick smear layer and debris after post space
preparation, which might be much more difficult to
remove with regular water irrigation, as recommended
by the manufacturer (16), because of the narrow and
deep circumstance of the post space.
Chemical irrigation has been recommended as a reg-
ular procedure for removal of the smear layer in root
canal treatments (17–19). In previous studies, alternate
irrigation with ethylenediaminetetracetic acid (EDTA)
and sodium hypochlorite (NaOCl) was effective in
598 Gu et al.
removal of the smear layer (19). However, such irrigation
might lead to severe erosion on the root canal dentin
surface (18, 20). The reported effects of irrigants on bond
strength are controversial. Wachlarowicz et al. (21)
demonstrated that endodontic irrigants, such as EDTA
and NaOCl, could significantly improve the bond
strength, whereas Ari et al. (22) and Santos et al. (23)
reported that NaOCl had adverse effects on the adhesive
bond strength. Therefore, it remains a challenge to
achieve the appropriate condition of root canal dentin
for effective bonding. To the author!s knowledge, only a
few studies have focused on the efficacy of smear layer
and debris removal using different irrigants after post
space preparation (16, 24). However, these studies lacked
data on the effects of the irrigants on the bond strength,
and only Zhang et al. (25) evaluated the effect of post-
space treatments on the retention of fiber posts and
found that ultrasonic agitation with EDTA/NaOCl irri-
gation improved the bonding strength of fiber posts in
the deep region.
The purpose of this study was to evaluate smear layer
removal, RDIZ, resin tags, and bond strength of the self-
etch adhesive bonding to root canal dentin, using different
irrigating solutions, and to test whether there is a rela-
tionship between smear layer removal and bond strength.
The null hypotheses tested were that the smear layer
removal, bond strength, RDIZ, and resin tag formation
would not be affected by irrigation of the post space with
different solutions, and that these factors do not vary
among coronal, middle, and apical thirds of the root.
Material and methods
Tooth preparation
After obtaining approval from the university ethics com-
mittee, 66 sound extracted single-rooted teeth, from 40–60-
yr-old patients with periodontal disease, were selected for
the study and stored in 0.1% thymol solution within
3 months after extraction. The patients were informed that
their teeth would be used for research and their written
consent for this was obtained. Endodontic treatment was
performed for all teeth chemo-mechanically. The root
canals were prepared through step-back filing to ISO size
60. After intermittent rinsing with 2.5% sodium hypo-
chloride, all root canals were obturated using a resin sealer
(AH plus; DeTrey, Constance, Germany) and lateral
condensation of gutta-percha points (Dentsply, York, PA,
USA). The teeth were then immersed in the freshly mixed
thymol solution for 2 wk (2).
The anatomic crown of each tooth was cut off at the line
2 mm incisally to the cemento–enamel junction. The gutta-
percha was removed and a post space was prepared using
low-speed post drills (Snowpost; Carbotech, Ganges,
France) to a length of 10 mm and a diameter of 1.6–
1.8 mm, depending on the tooth size, leaving more than
4 mm of gutta-percha to preserve the apical seal. All teeth
were then randomly assigned to three groups of 22 teeth
each, and irrigated respectively as follows.
Group 1: irrigated with 14% EDTA for 60 s.
Group 2: irrigated with 5.25% NaOCl for 60 s.
Group 3: irrigated with 0.9% sodium chloride (NaCl) for
60 s. This group served as a negative control.
Smear layer evaluation
Eight of 22 teeth in each group were split longitudinally
along the labio–lingual surfaces after irrigation. These
halved specimens were dehydrated in an ethanol series (50%,
75%, 95%, 100%) and then dried in a desiccator for 24 h.
After sputter-coating with gold palladium, each specimen
was examined using a field-emission scanning electron
microscope (FE-SEM, S-4800; Hitachi, Tokyo, Japan) at
1-, 4.5-, and 8-mm levels from the apical to the coronal third
of the post space. Twenty serial fields of vision were observed
and marked, in a blind manner and separately, by two
investigators, at 1000· magnification at each level for each
tooth, according to the criteria shown in the list below (24).
Field-emission scanning electron micrographs of each level
were taken at 1000· and 2000· original magnifications.
The amount of debris observed at 1000· magnification
was marked from 0 to 2, as follows:
Mark 0: no debris particles;
Mark 1: a few debris particles, with maximum diameter of
less than 20 lm; and
Mark 2: large amounts of debris particles, with diameter
greater than 20 lm in any direction.
Observation of RDIZ and resin tags
After irrigation of the post space and thorough rinsing with
water, 4 of 22 teeth in each group were ready for RDIZ and
resin tag analyses. A self-etching adhesive resin luting sys-
tem (Panavia F, batch no. 71127; Kuraray, Osaka, Japan,)
was selected as the cement. According to the manufacturer!s
instructions, the post space of each tooth was dried lightly
with paper points, after which ED primer was applied to the
root canal dentin walls with a microbrush (Microbrush,
Greyton, WI, USA) and gently dried with paper points and
oil-free air for 60 s. Then, the mixed luting cement was
injected into the post space using a disposable metal tip.
After carefully removing excess cement, the surface of the
cement and the cement–dentin interface were covered with
Oxyguard II (Kuraray) for 3 min. All filled roots were stored
in deionized water at 37"C for 1 wk before observation.
The roots were then sectioned longitudinally in the labio–
lingual direction using a low-speed diamond saw (Isomet
1000; Buehler, Lake Bluff, IL, USA). One section of each
root was gently decalcified (in 35% phosphoric acid for
30 s) and deproteinized (in 2% sodium hypochlorite solu-
tion for 120 s) for RDIZ evaluation. The other section was
immersed in a solution of 30% HCl for 24 h, which com-
pletely dissolved the dental substrate, allowing resin tags to
be observed. The specimens were dehydrated, dried, and
then examined using FE-SEM, as described above.
Push-out test
The remaining 10 teeth of each group were used for the
push-out test. In order to ensure that the push-out force was
applied on the resin cement cylinder longitudinally, the post
drill was mounted to a paralleling fixture and the root was
attached to a positioner by wax, to ensure that each root
was sectioned perpendicularly. After irrigation of the post
space, the post space of each tooth root was filled with
Panavia F resin cement, as described above. All specimens
were then stored in deionized water at 37"C for 1 wk.
The root was serially sectioned from 1 mm below the
coronal surface to the apex, transversally using a low-speed
diamond saw (Isomet 1000; Buehler). Six, 1-mm-thick serial
 Smear layer removal and bonding 599

sections were obtained and divided into two coronal, mid- A

dle, and apical portions each, respectively. The sections were
then tested using a universal testing machine (Z010/TN2S;
Zwick, Ulm, Germany), with the apical surface upwards, at
a cross-head speed of 0.5 mm min)1. The section was loa-
ded until bond failure, and the maximum failure load was
recorded. Cylindrical post drills with a long apical cone
(Snowpost) were used in the study, so the bond strength
(MPa) was calculated according to the following formula:
r ¼ F=pðr1 þ r2 Þh;
50.0 µm

where r1 and r2 represent the diameters of the two different

B
cement surfaces respectively, h represents the height of the
segment, and F represents the maximum failure load.

Evaluation of failure modes

After performing the push-out test, all specimens were
assessed using a microscope (Nikon 80i; Nikon, Tokyo,
Japan), at 50· magnification, to determine the type of
failure mode. The failure modes were classified into the
following categories: type I, adhesive failure between den- 50.0 µm
tin and resin cement; type II, cohesive failure within resin
cement; type III, cohesive failure within dentin; and type C
IV, mixed failure (partial adhesive failure with a thin layer
of resin cement remaining on the dentin surface). Speci-
mens with adhesive failure were decalcified (in 35% phos-
phoric acid for 30 s) and deproteinized (in 2% sodium
hypochlorite solution for 120 s), before examining the
debonded interface using scanning electron microscopy at
1000· magnification.

Statistical analyses 50.0 µm

For each tooth, the mean marks of smear layer and debris
were calculated separately for the three regional portions of
the root canal dentin (i.e. coronal, middle, and apical third).
The final results of smear layer and debris marks were
analyzed statistically using the Kruskal–Wallis H-test and
the Mann–Whitney U-test with a P-value of £ 0.05.
The measurements of push-out bond strength were
pooled for the regional portions in each group. The
Kolmogorov–Smirnov test was used to determine whether
data were normally distributed. Because of non-normal
distribution of the data among groups, a multivariate
statistical analysis was not applied. The differences between
the coronal, middle, and apical portions in each group, and
the differences between the groups at each portion, were
analyzed using the Kruskal–Wallis H-test and the Mann–
Whitney U-test with a P-value of £ 0.05. The percentage
of each failure mode within each group was calculated.
Results
Smear layer evaluation
Removal of the smear layer from the root canal surface
was significantly affected by irrigation of the post space.
The morphological changes and smear layer marks are
shown in Fig. 1.
In the EDTA group, smear layer and debris were
removed completely along the entire root canal dentin
surface, and no significant difference was found among
the coronal, middle, and apical thirds of the post space.
Fig. 1. Scanning electron micrographs (1000· magnification)
showing the radicular dentin surface cleaned with different
irrigants. (A) Ethylenediaminetetracetic acid (EDTA) group: no
smear layer visible and most dentinal tubules open. (B) Sodium
hypochlorite (NaOCl) group: debris remained and all dentinal
tubules blocked. (C) The control [sodium chloride (NaCl)
group]: a heavy smear layer covered the dentin surface and no
dentinal tubules were visible.
In the NaOCl group, the smear layer was removed
mostly at the coronal and middle thirds, but remained at
the apical third. However, the dentinal tubules were
blocked with debris and were not fully open along the
entire root canal dentin surface. Significantly more smear
layer and debris was present at the apical third than at
the coronal (P £ 0.01) and middle thirds (P < 0.05).
The surfaces of specimens irrigated with NaCl were
covered with a heavy smear layer along the entire post
space, and no open dentinal tubules were observed. No
significant differences were found among the coronal,
middle, and apical thirds in the NaCl group.
With regard to the difference between the three irri-
gation groups, statistical analyses revealed that EDTA
was significantly more effective at removing the smear
layer than NaOCl or NaCl at each regional third of the
post space (P £ 0.01). The statistical significance of
dentinal tubule opening was in accordance with those of
smear layer and debris removal (Fig. 2).
600 Gu et al.

50.0 µm

B
Fig. 2. Marks of smear layer and debris at three levels of root
canal dentin surface after three different irrigations. Ethylen-
ediaminetetracetic acid (EDTA) was significantly more effective
at smear layer removal than either sodium hypochlorite
(NaOCl) or sodium chloride (NaCl) at each region of the tooth
(apical, middle, and coronal) (P £ 0.01). The top horizontal
lines connect values that are not statistically significantly
different.

50.0 µm

RDIZ and resin tag observation C

Resin tag formation and RDIZ differed between the

three irrigant groups. The typical morphological results
are shown in Figs 3 and 4. In the EDTA group, uniform
RDIZ were formed, and no gaps could be detected along
the entire interface. Resin tags were observed from the
coronal to the apical portion. Most tags were 20–30 lm
long and frequent lateral branches could be seen in the
coronal third. In NaOCl and NaCl groups, RDIZ was
not homogeneous along the entire root. Fewer and
shorter resin tags were found, which were irregularly
distributed and of different lengths.
Push-out test
In general, the push-out bond strength was significantly
affected by the different irrigants. Figure 5 presents the
bond strength of the three groups at each tooth portion
analyzed (i.e. coronal, middle, and apical). The bond
strengths in the EDTA group were significantly higher
than the bond strengths in the NaOCl and NaCl groups
at each portion (P £ 0.01 at the coronal and apical
thirds, P £ 0.05 at the middle third). Overall, the mean
bond strength in the NaOCl group was lower than in the
NaCl group; however, the differences between these
groups at each portion were not significant. Within each
irrigant group, no significant differences were found
between the bond strengths of the coronal, middle, and
apical portions.
Evaluation of failure modes
Failure modes of each group are shown in Fig. 6. More
than 90% of the failures in each group were adhesive
failures between dentin and resin cement, or were mixed
failures. Cohesive failures within the resin cement
occurred only rarely. No cohesive failures within the
dentin were observed in this study. The morphological
observation showed that adhesive failures occurred
50.0 µm
Fig. 3. Scanning electron micrographs (1000· magnification) of
the resin dentin interdiffusion zone (RDIZ) and resin tag
formation in three different groups. (A) Ethylenediaminetetr-
acetic acid (EDTA) group. (B) Sodium hypochlorite (NaOCl)
group. (C) The control [sodium chloride (NaCl)] group.
mostly along the hybridized smear layer with cohesively
fractured resin tags (Fig. 7).
Discussion
The results of the current study showed that EDTA
could effectively remove both smear layer and debris
from the dentin surface and the dentinal tubules along
the entire post space. These results are in agreement with
the findings of Perez-Heredia et al. (26) after endodontic
instrumentation, and may be attributed to the low pH of
EDTA, which acts as a calcium chelator, resulting in
demineralization of the root canal dentin surface (27).
Previous studies have revealed that irrigation with a
high concentration of NaOCl enhances cleanliness of the
root canal (28), and 5.25% NaOCl has been widely used
for smear layer removal (18, 20, 29). However, the
efficacy of NaOCl on smear layer removal remained
questionable. In the present study, smear layer removal
was less effective in the NaOCl group than in the EDTA
group but was more effective than in the NaCl group.
 Smear layer removal and bonding 601

50.0 µm

B
Fig. 5. Push-out bond strength (MPa) at three levels (coronal,
middle, and apical) of post space after irrigation with one of
three different solutions. The bond strength in the ethylene-
diaminetetracetic acid (EDTA) group was significantly higher
than that of the sodium hypochlorite (NaOCl) and the sodium
chloride (NaCl) group at each level (P £ 0.01 at coronal and
apical levels, and P £ 0.05 at the middle level). The top
horizontal lines connect values that are not statistically
significantly different.
50.0 µm

50.0 µm

Fig. 4. Scanning electron micrographs (1000· magnification) of

the resin tags after complete dissolution of the dental substrate.
(A) Ethylenediaminetetracetic acid (EDTA) group: most of the
tags were up to 20–30 lm and lateral branches were observed. Fig. 6. Failure modes of test groups. EDTA, ethylenediamin-
(B) Sodium hypochlorite (NaOCl) group and (C) the control etetracetic acid; NaCl, sodium chloride; NaOCl, sodium
[sodium chloride (NaCl)] group: fewer and shorter resin tags or hypochlorite.
only resin plugs were observed.

These results are in contrast to the findings of

Torabinejad et al. (18), who reported that NaOCl was
ineffective in removing the smear layer from the root
canal dentin surface after endodontic instrumentation.
This finding might be explained by the lower surface
tension value of NaOCl compared with NaCl (30). An
irrigant with low surface tension might improve the
dentin wettability, and thus flow into root canals and
contact with the dentin and the smear layer effectively
(31, 32). Moreover, NaOCl might have partially removed
the smear layer by resolving the organic composition,
while NaCl cannot achieve effective removal of the smear
layer. Fig. 7. Scanning electron micrograph of a debonded specimen
with adhesive failure mode. Failure occurred along the
Bonding effectiveness hybridized smear layer, which showed cohesively fractured
resin tags.
In the current in vitro study, the irrigated post space was
filled with a self-adhesive resin luting cement, without the
use of fiber posts, to evaluate the effect of the irrigants on root canal dentin without fiber posts. Although it must
the resin bond strength. Pest et al. (33) also evaluated be admitted that absolute bond strength values might
the push-out bond strength between resin cement and have differed upon the addition of posts, it can be
602 Gu et al.
assumed that the ranking of the groups would be the
same. The adhesive failure mode between the resin
cement and dentin was the main failure mode. This
shows that the test design of the current study was able
to test the strength at the bonded resin–dentin interface
in an accurate manner.
The push-out bond strength of the EDTA group was
significantly higher than those of other two groups. This
result is supported by other researchers (34, 35), who
revealed that previous treatment with EDTA increased
the bond strength of self-etching adhesive systems. In
accordance with the push-out bond strength, apparently
homogeneous RDIZ and uniform resin tags were formed
when irrigated with EDTA. As a mild chelating agent,
EDTA could remove the hydroxyapatite and non-
collagenous protein selectively, avoiding major altera-
tions of the native collagen fibrillar structure (36, 37). As
the unaltered collagen fibrils are thought to preserve
most of their intrafibrillar mineral, they are more stable
and less affected by dehydration (37), which subse-
quently improves the infiltration of the resin materials.
Therefore, stable mechanical interlocking between resin
cement and dentin occurred, resulting in higher bond
strength.
The results of the current study showed that NaOCl
had adverse effects on the bond strength. The push-out
bond strength in the NaOCl group was lower than in the
NaCl group, although the difference was not significant.
This result is in accordance with other findings that
irrigation with NaOCl could reduce the resin–dentin
bond strength (22, 23). Micromorphological investiga-
tions showed that in the NaOCl group, less apparent
resin tags and inferior RDIZ were formed. NaOCl is
capable of removing the organic components of dentin,
including collagen fibrils (37). Also, it might modify the
properties of collagen, including structure and suscepti-
bility to proteolysis (38). These alternations of the
collagen fibrils might be responsible for bond strength
reduction (39). In addition, the release of oxygen from
NaOCl might inhibit the interfacial polymerization of
resin cements (40). Reductions in elastic modulus and
microhardness after irrigation with NaOCl might also
contribute to the decrease in micromechanical interac-
tion between resin cement and dentin (41), which resulted
in a reduction of the bond strength.
No significant differences of push-out bond strength
were found between the different regional portions of the
root canal in the current study. This is in agreement with
the results of other studies (6, 25). However, Wang et al.
(42) reported that the bond strength at the apical level of
the root canal was significantly lower than those at other
levels, and such a result was caused by different distri-
butions and densities of dentinal tubules in different root
regions. In our opinion, these controversial findings also
indicated that the luting procedure in the narrow and
deep post space was difficult to control. In the current
study, a thin microbrush was used to carry ED primer
deep into the post space and to assure even coating. Such
usage of a microbrush was confirmed to be more useful
and effective than usage of a standard brush (43). This
might be a reason why the bond strength did not sig-
nificantly decrease from the coronal to the apical third of
the root.
In the current study, push-out failures mostly occurred
at the cement–dentin interface, along the hybridized
smear layer, indicating that this zone was a potential
weak link in the bonding interface (14). This result sug-
gested that smear layer removal plays an important role
in bond strength. As the dentin surfaces in groups
NaOCl and NaCl were covered with smear layer and
debris, which act as a diffusion barrier and reduce
the dentin permeability (4, 44), this might have prevented
the infiltration of the ED primer and the luting resin into
the dentinal tubules.
Within the limitations of this in vitro study, it can be
concluded that different irrigants have significantly
different effects on smear layer removal and bonding
effectiveness after post space preparation. EDTA
removed the smear layer extremely effectively and, as a
result, increased the bond strength. Irrigation with
EDTA after post space preparation is therefore a valu-
able procedure when a self-etching adhesive resin luting
system is used for fiber post cementation.
Acknowledgments – This investigation was supported by the
Science and Technology Program of Zhejiang Province (grant
no. 2009C33094) and the Medical and Health Science Foun-
dation of Zhejiang Province (grant no. 2007A061).
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