Basic Research—Technology
Soft Chelating Irrigation Protocol Optimizes Bonding
Quality of Resilon/Epiphany Root Fillings
Gustavo De-Deus, MS,* Fátima Namen, PhD,* João Galan Jr, PhD,*
and Matthias Zehnder, PhD†
Abstract
This study was designed to test the impact of either
a strong (MTAD) or a soft (1-hydroxyethylidene-1,
1-bisphosphonate [HEPB]) chelating solution on the
bond strength of Resilon/Epiphany root fillings. Both
17% EDTA and the omission of a chelator in the
irrigation protocol were used as reference treatments.
Forty extracted human upper lateral incisors were pre-
pared using different irrigation protocols (n ⫽ 10): G1:
NaOCl, G2: NaOCl ⫹ 17% EDTA, G3: NaOCl ⫹ BioPure
MTAD (Dentsply/Tulsa, Tulsa, OK), and G4: NaOCl ⫹
18% HEPB. The teeth were obturated and then pre-
pared for micropush-out assessment using root slices of
1 mm thickness. Loading was performed on a universal
testing machine at a speed of 0.5 mm/min. One-way
analysis of variance and Tukey multiple comparisons
were used to compare the results among the experi-
mental groups. EDTA- and MTAD-treated samples re-
vealed intermediate bond strength (0.3–3.6 MPa). The
lowest bond strengths were achieved in NaOCl-treated
samples (0.3–1.2 MPa, p ⬍ 0.05). The highest bond
strength was reached in the HEBP-treated samples
(3.1– 6.1 MPa, p ⬍ 0.05). Under the present in vitro
conditions, the soft chelating irrigation protocol (18%
HEBP) optimized the bonding quality of Resilon/Epiph-
any (Resilon Research LLC, Madison, CT) root fillings. (J
Endod 2008;34:703–705)
Key Words
Adhesive root filling, chelating solution, EDTA, Epiphany,
final rinse, irrigation, MTAD, Resilon, smear layer,
1-bisphosphonate, 1-hydroxyethylidene-1
*From the Veiga de Almeida University, Rio de Janeiro,
Brazil; and †Division of Endodontology, Department of Pre-
ventive Dentistry, Periodontology, and Cariology, University of
Zürich Center for Dental Medicine, Zurich, Switzerland.
Address requests for reprints to Dr Gustavo De-Deus,
R. Desembargador Renato Tavares, 11, ap.102-Ipanema,
Rio de Janeiro, Brazil. E-mail address: endogus@gmail.com.
0099-2399/$0 - see front matter
Copyright © 2008 by the American Association of
Endodontists.
doi:10.1016/j.joen.2008.02.024
JOE — Volume 34, Number 6, June 2008
T he introduction of the polycaprolactone-based core filling material Resilon (Resilon
Research LLC, Madison, CT) to the dental market has recently resurrected the
adhesive root-filling issue. Early reports on the improvement of both seal quality and
root fracture resistance in comparison to gutta-percha and conventional sealer (1, 2)
advocated the use of Resilon/Epiphany (Resilon Research) adhesive root fillings. How-
ever, more recent and independent studies have yielded unfavorable results (3– 6).
The message based on the accumulated knowledge of adhesive dentistry research
is clear; bonding to a wet substrate such as root dentin is a difficult task (7, 8). For
optimal results, the mineral phase of the dentin needs to be efficiently replaced by an
adhesive, which will permeate into the collagen-rich web forming the so-called hybrid
layer (9). To obtain optimal bonding, dentin pretreatment is crucial (10, 11). In
current endodontic practice, combinations of decalcifying agents and sodium hypo-
chlorite have been recommended to chemically clean the root canal system. However,
the sequential use of EDTA and NaOCl caused a progressive dissolution of dentin at the
expense of peritubular and intertubular areas (12–14). Regarding the adhesive filling
approach, there is an ongoing debate on the ideal extent of the smear removal. There is
uncertainty at this point as to whether strong or weak decalcifying agents should be
used. Strong agents completely remove the inorganic aspects of the smear layer but bear
the disadvantage that they attack the dentin and may thus hamper its mechanical prop-
erties (14 –16). Moreover, the increase in the tubular dentin area as well as the con-
sequent reduction of the intertubular dentin promoted by strong chelating agents is
unfavorable for bonding (7). So, a moderate decalcifying effect may represent a good
choice in case the prevention of the peritubular and intertubular dentin is desired (17).
Recent studies have reported the negative effects of endodontic irrigants on bond
strengths of resinous materials to dentin (10, 18, 19). Therefore, the appropriate
conditions of radicular dentin to optimize the quality of bonding need to be determined.
To understand the influence of the dentin demineralization promoted by different canal
irrigation protocols on the quality of adhesive root fillings, we used a micropush-out
bond strength model. This study was designed to test the null hypothesis that the use of
either a strong (MTAD) or a soft (1-hydroxyethylidene-1, 1-bisphosphonate (HEBP),
also known as etidronic acid or etidronate) chelating solution does not have a signifi-
cant impact on the bond strength of Resilon/Epiphany root fillings. Both 17% EDTA and
smear-covered dentin were used as reference treatments to compare the results.
Materials and Methods
Specimen Preparation
Forty extracted human upper lateral incisors that were 20 ⫾ 1 mm in length and
had straight roots were selected from the tooth bank of Veiga de Almeida University. This
study was revised and approved by the Ethics Committee, Nucleus of Collective Health
Studies of Veiga de Almeida University. The teeth were disinfected in 0.5% chloramine
T, stored in distilled water at 4°C (20), and used within 6 months after extraction.
The teeth were randomly distributed with the aid of a computer algorithm (http://
www.random.org) into 4 similar experimental groups (n ⫽ 10).
Standard access cavities were made, the patency of each canal was confirmed,and
the working length was established by deducting 1 mm from the canal length. The root
canal was prepared using K3 NiTi rotary instruments (SybronEndo, West Collins, CA) at
250 rpm. The final preparation has a 0.06 taper with a diameter of 0.35 mm at the apex.
Irrigation was performed by using a 5-mL disposable plastic syringe (Ultradent Prod-
Soft Chelating Irrigation Protocol Optimizes Bonding 703
Basic Research—Technology
ucts Inc., South Jordan, UT) with a polypropylene capillary tip (Ultra-
dent) placed passively into the canal up to 3 mm from the apical fora-
men without binding.
In G1, the canals were irrigated between each filing with 0.5 mL of
freshly prepared 1.25% NaOCl, with no final flush to remove the smear
layer. The specimens of G2 were prepared similar to those of G1, with
the exception that the smear layer was removed by a flush of 3 mL of 17%
EDTA (pH 7.7; Herpo Ltd, Petrópolis, RJ, Brazil) for 3 minutes. In G3,
canals were irrigated between each file with 0.5 mL of freshly prepared
1.25% NaOCl and 5 mL of BioPure MTAD (Dentsply/Tulsa, Tulsa, OK)
for 5 minutes. In G4, 0.25 mL of 18% HEBP (etidronate; Zschimmer &
Schwarz Mohsdorf GmbH & Co KG, Burgstädt, Germany) mixed with
0.25 mL of 1.25% NaOCl were used between each file. In addition, 2 mL
of 18% HEBP were used after the mechanical preparation for 2 minutes
(17, 21). A final rinse of 3 mL of sterile water was performed in all
groups. The NaOCl solution was prepared by diluting a 10% NaOCl
solution (Merck SA, São Paulo, SP, Brazil). Its pH was adjusted to 10.8
with 1 N HCl. The concentration of the NaOCl solution was measured
iodometrically.
Canal Filling
The prepared teeth were filled by using the passive-fit single-cone
obturation protocol in order to control the methodological variables
associated with the filling technique (22). Following the manufacturer’s
directions, Epiphany self-etching primer was introduced into the canals
for 1 minute using a microbrush. The excess primer was removed with
paper points. A prefitted size 35 0.06-taper Resilon cone (Resilon Re-
search LLC) was galore coated with Epiphany sealer was then insert at
the working length. To create the immediate coronal seal of Reslion/
Epiphany, the teeth were light cured for 40 seconds with a Coltolux LED
curing light (Coltene Whaledent Product, Cuyahoga Falls, OH).
The crowns of all specimens were removed, leaving roots that were
11 mm in length. The filled roots were stored at 37°C and 100% hu-
midity for 7 days to allow setting of the sealer.
Micropush-out Assessment
Each root was horizontally sectioned into nine 1 ⫾ 0.1 mm thick
serial slices by using a low-speed saw (Isomet; Buhler, Ltd Lake Bluff,
NY) with a diamond disk (A 125 mm ⫻ 0.20 mm ⫻ 12.7 mm, 33°C)
under continuous water irrigation. The thus-created nine slices per root
resulted in 90 slices/group or 30 slices per root segment (coronal,
middle, and apical).
The thickness of each slice were measured with a digital caliper
with an accuracy of 0.001 mm (Avenger Products, North Plains, OR),
and it was always within the 0.9 to 1.1 mm range. Then, both the apical
and coronal aspects of the specimens were microscopically examined
before testing to confirm a circular canal shape. The fine-tune parallel-
ism was ensured by a laser beam device, and the root filling of each
sample was loaded with a 0.5-mm diameter cylindrical plunger. The
plunger tip was sized and positioned to touch only the root filling. The
load was applied always in an apical-coronal direction to avoid any
constriction interference because of the root canal taper during push-
out testing. Loading was performed on a universal testing machine
(EMIC DL200MF, São José dos Pinhais, PR, Brazil) at a speed of 0.5
mm/min until debonding occurred. A curve during compression testing
load/time was plotted during the test by using a real-time software
program. In order to express the bond strength in MPa, the load at
failure recorded in Newtons was divided by the area of the bonded
interface.
The normally distributed data (Kolmogorov-Smirnov test) were
analyzed by one-way analysis of variance. Post hoc pair-wise compari-
704 De-Deus et al.
Figure 1. Boxplots of the micropush-out bond strength data. Letters indicate
significant differences between groups; p ⬍ 0.05.
sons were performed using Tukey multiple comparisons. The level of
significance was set at p ⬍ 0.05.
Results
The root fillings in all groups showed measurable adhesive prop-
erties. The group-by-location interaction was not significant (p ⫽
0.75), and thus the group comparisons were not dependent on the
canal third. As a consequence, data from the 3 root thirds were pooled
to provide a single mean and standard deviation per irrigation protocol,
averaging 10 teeth per group.
EDTA- and MTAD-treated samples revealed intermediate bond
strengths (0.3–3.6 MPa) that were not significantly different from each
other (p ⬎ 0.05). The lowest bond strengths were achieved in NaOCl-
treated samples (0.3–1.2 MPa). These values were significantly lower
than those observed in the others 3 groups (p ⬍ 0.05). The highest
bond strength was reached in the HEBP-treated samples (3.1– 6.1 MPa)
(p ⬍ 0.05). Boxplots in are shown in Figure 1.
Discussion
Our results showed that HEBP-treated dentin displayed a more
effective bonding than EDTA-, NaOCl- and MTAD-treated dentin. There-
fore, the null hypothesis was rejected.
In theory, the low push-out strength values in NaOCl-treated spec-
imens have a two-fold origin: the presence of smear layer as well as the
strong oxidizing NaOCl effect. Several studies have underlined that ex-
posure to NaOCl results in reduced resin bond strengths (23, 24).
However, because a final rinse of sterile water was applied in all groups
of the current study, the compromising effect of NaOCl on sealer poly-
merization should be negligible (23, 24). Consequently, it is more likely
that the sealer bonded to the inorganic aspects of the smear layer rather
than the dentin proper in the NaOCl-only group (G1), and thus root
fillings showed little resistance to push-out forces.
It has been suggested that the smear-removal procedures allow the
sealer penetration into the dental tubules and thus could increase the
dentin bond strength of resin-based sealers as well as an enhanced seal
(25, 26). However, contrary to the common belief, the dentinal tubules
have just a minor contribution to the dentin adhesion process with
self-etch adhesive systems (7). The major retention is provided by mi-
cromechanical interactions of the bonding agent with the collagen ma-
trix and the underlying mineralized zone in the intertubular dentin (27,
JOE — Volume 34, Number 6, June 2008

28). Thus, the total available area of intertubular dentin is an important
aspect in this so-called hybridization process. We believe that this point
can be correlated with the best performance found in HEBP-treated
dentin. Recently, De-Deus et al. (17) using a co-site single-tooth com-
parative model have displayed the soft chelating ability of 18% HEBP
solution. A comparatively greater dentin tubular area was achieved in
EDTA- and MTAD-treated specimens. So, we can assume that a larger
intertubular dentin area is available for hybridization when a soft che-
lating irrigation protocol is applied.
Another possibly positive aspect pertaining to the use of a soft
chelating solution is the depth of demineralization. The complete infil-
tration of resin-based sealer into the demineralized dentin is a hard task
because of the difficulty of resin infiltration through a collapsed collagen
matrix (7, 10). If the resin does not completely infiltrate, fluid move-
ment between the hybrid layer and unaffected dentin expedites bond
degradation (29 –31). That way, the depth of the demineralized zone is
a critical factor. Garcia-Godoy et al. (10) showed that the EDTA-created
demineralized-dentin zone was 2 to 4 ␮m deep, whereas the corre-
sponding MTAD-created zone was 8 to 12 ␮m. Because the current
endodontic practice aims at a smear-free dentin, these authors detected
“. . . a possible dilemma between the currently accepted endodontic
filling concepts and the modern principles of dentin bonding” (10). In
other words, powerful chelators such as EDTA and the citric acid con-
tained in MTAD produce a demineralized dentin zone too deep to allow
effective adhesive infiltration (10). A further point that can intensify this
condition is the acidic nature of the Epiphany primer (pH 1.5) (31). If
the manufacturer’s instructions are exactly followed (32), it is likely that
the Epiphany primer enhances the demineralized dentin zone produced
by the chelators. This prolonged etching time can result in a suboptimal
infiltration of the adhesive into the demineralized dentin resulting in a
weak bond and accelerated degradation (7, 10). This rationale is in
agreement with Van Landuyt et al. (33) who reported reduced bond
strengths with “mild” self-etch primers as well as an inferior quality of
the hybrid layer when dentin is demineralized by a strong acid before-
hand.
In summary, the present study showed the influence of different
chelators on the quality of the bonded root fillings. Under the present in
vitro conditions, a soft chelating irrigation protocol optimizes bonding
quality of Resilon/Epiphany root fillings. Although the bond strength to
dentin is an important step to maintaining the integrity over time (34 –
36), it is only one of the noteworthy facets regarding the quality of
adhesive root fillings. Further investigations are needed to clarify the
quality of the effect of the use of a soft chelating irrigation protocol on
other important features of adhesive root fillings, such as their ability to
prevent microbial recolonization of the root canal system and their
long-term integrity.
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