EFFECT OF 0.

2% CHITOSAN SOLUTION ON THE PULL-OUT BOND STRENGTH

OF GLASS FIBER POSTS BONDED WITH DIFFERENT CEMENTS

Abstract:
Objective: To evaluate the effect of 0.2% chitosan conditioning upon the pull out
bond strength of posts bonded with different cements.
Materials and Method: Sixty freshly extracted human permanent canines
with single roots were selected, instrumented with Rotary ProTaper in a
sequential manner till F4 and obturated. The post space was prepared to a
depth of 12 mm using No. 1-3 drills of the glass fibre post system. Samples
were randomly divided into 2 groups (n=30) on the basis of chelators used.
Group A: 5 ml of 17% ethylenediaminetetraacetic acid (EDTA) for 3 minutes.
Group B: 5 ml of 0.2% chitosan for 3 minutes. Each group was randomly
divided into two equal sub-groups on the basis of luting cement. Group A1
and B1: Dual-Cure resin cement: RelyX U200. Group A2 and B2: Dual-Cure
resin cement: SmartCem 2. After the cementation, the pull out bond strength
of posts was tested with universal testing machine at a rate of 0.5mm/min until
the posts separated. The results, in newtons, were analyzed with 1-way
ANOVA and independent t test ( = .01).
Results:

Highest mean pull out bond strength was observed for sub-group A1

(312.20 N) and lowest for sub-group A2 (133.47). Statistically significant difference

(p<0.01) was observed in the mean pull out bond strength values of all the subgroups except for sub-groups A2 and B2.

Conclusion: The type of chelator used for post space conditioning significantly
affected pull out bond strength of glass fibre posts.
Keywords: Chitosan, EDTA, Fibre glass posts, Pull-Out Bond Strength, Selfadhesive resin cements.
INTRODUCTION
Restoration of endodontically treated teeth is often complicated because of the loss
of tooth structure by caries, restorative procedures, fractures, and endodontic access
preparation. All of these have a negative impact on a large part of the crown
structure, resulting in the need for the use of intra-radicular posts, with the aim of
increasing stability and resistance to the fracture. 1,2
Fibre reinforced resin posts have gained popularity in the last few years to restore
endodontically treated teeth. They consist of epoxy resin matrix with reinforcing glass
or quartz fibre. Important characteristics include modulus of elasticity similar to that
of dentin, ability to be cemented using an adhesive technique, superior distribution of
masticatory forces, biocompatibility, high durability, resistance to corrosion and
esthetically superior as their optical properties provide greater translucency to the
dental core.1,2
Clinical studies3,4 have reported success rates of 95 to 99% for teeth restored with
fibre-reinforced posts. The retention of fibre posts in the root canal depends on the
bond strength between the post material and a luting agent, as well as the bond
strength between the luting agent and post space dentin. 5-8 However, failures have
been reported in the form pull out of the cement and/or post restoration assembly, as
a result of lack of retention of the fibre posts. 9,10

The recent trend for luting fibre posts has been toward resin cements, because they
increase retention, tend to leak less than other cements and provide at least shortterm strengthening of the root.11 However, they are more technique sensitive and
require extra steps such as pretreatment or conditioning of the canal walls with acid
or EDTA and placing a dentin-bonding agent. 11
To overcome these limitations self-adhesive cements were introduced in 2002.
These cements do not require separate steps of etching and bonding and their main
adhesive mechanism is attributed to a chemical reaction between phosphate
methacrylates and hydroxyapatite.12
Retention of adhesive luting agents to the root canal dentin is based on several
factors of which smear layer is one of the factors. Studies have suggested that the
efficacy of the dentin adhesive mostly depends on the removal of the smear layer. 13,14
Chemical irrigation has been recommended as a regular procedure for removal of
smear

layer

in

root

canal

treatments.15

Alternate

irrigation

with

ethylenediaminetetracetic acid (EDTA) and sodium hypochlorite (NaOCl) has shown

effective results.16
EDTA is a divalent cationic material used to chelate calcium ions as a part of an
endodontic therapy procedure.17 It improves the retention of post by removing the
smear layer, opening the dentinal tubules, and/or etching the inter-tubular dentin thus
improving contact between the luting cement and the dentin. 18 EDTA also enhances
the mobility and bioavailability of heavy metals and has poor bio-degradability thus
has environmental concerns. 19
Chitosan is a natural polysaccharide, prepared by the deacetylation of chitin, which
is obtained from the shells of crabs and shrimps. This polysaccharide is endowed
3

with properties of biocompatibility, biodegradability and bio-adhesion in addition to its

high chelating capacity for different metallic ions. 20 The chitosan solution acts on the
inorganic portion of the smear layer, favouring its removal. However, the effect of
chitosan as an endodontic irrigant on the bond strength of endodontic posts and
luting cements has not yet been established. Hence, the purpose of this study was to
evaluate the effect of 0.2% Chitosan conditioning on the bond strength of glass fibre
posts bonded with different resin cements.
MATERIALS AND METHODS
Freshly extracted human permanent maxillary and mandibular canines extracted for
periodontal reasons were selected and cleaned of calculus and organic debris. Sixty
teeth with single, straight, mature roots with cervical diameter of 6-6.5 mm in
mesiodistal direction and 9-9.5 mm in buccolingual direction were selected and
stored in 1% chloramine-T solution until use. Length of all the specimens was
standardized by resecting the crown at a distance of 17 mm from root tip. The
working lengths were established and biomechanical preparation was carried out
using rotary ProTaper Universal root canal files (S1-F4) (DENTSPLY Maillefer,
Ballaigues, Switzerland) according to manufacturers instructions. 1 ml of 5.25%
sodium hypochlorite was used to irrigate the canals after each instrumentation.
Obturation was carried out in both the groups using F4 ProTaper gutta-percha points
and AH plus sealer (DENTSPLY, De Trey, Germany). Excess gutta-percha was
seared off with a hot burnisher and was compacted vertically with finger pluggers.
Access cavities were temporised with 3 mm of Cavit-G and specimens were stored
in an incubator at 37C for 24 hours to allow complete setting of the sealer. The post
space was prepared to a depth of 12 mm using No. 1-3 drills of the glass fibre post
system (Reforpost, ANGELUS, Londrina, PR, Brazil). The resultant post space was
4

12 mm deep and 1.5 mm in diameter at apical end. Complete removal of gutta

percha from post space and complete seating of # 3 fibre post (Reforpost,
ANGELUS, Londrina, PR, Brazil) in the post space was verified radiographically and
clinically.
Specimens were divided into 2 groups (n=30) based on the chelator used for
removal of smear layer.
Group A: 17% ethylenediaminetetraacetic acid solution (EDTA) (PREVEST Ltd,
Jammu, India)
Group B: 0.2% Chitosan solution (ACROS ORGANICS, Belgium)
Irrigation was carried out with 5 ml of chelator for 3 minutes in the respective groups.
0.2% Chitosan solution was prepared by dissolving 0.2 gm of Chitosan powder in
100 ml of 1% acetic acid. The mixture was agitated using magnetic stirrer for 2 hours
and the pH was adjusted to 3.2 by buffering with sodium bicarbonate solution. (silvia
et al.)
The specimens in respective groups were randomly divided into two equal subgroups on the basis of the dual cure self-adhesive system used for post cementation.
Group A1 and B1: RelyX U200 (3M ESPE, St. Paul, MN, USA)
Group A2 and B2: SmartCem 2 (DENTSPLY Caulk, Milford, USA)
The posts were degreased using 96% alcohol and subsequently treated with Silane
(ANGELUS, Londrina, Brazil) over the entire surface for 1 minute.
Specimens in subgroup A1 and A2 were conditioned with 17% EDTA for 3 minutes to
remove the smear layer created during post space preparation. Similarly in

subgroups B1 and B2, the post spaces of the specimens were conditioned by
irrigating with 0.2% Chitosan solution for 3 minutes. The post spaces were then
rinsed copiously with 5 ml of distilled water to remove remnants of chelators. For
cementation of silanized post, the cement was manipulated according to the
manufacturers instructions. The cement was dispensed directly into the prepared
post space beginning apically in the root canal. The post was then covered with a
layer of cement and seated in the root canal immediately. Excess was removed with
a cotton pellet and the entire assembly was light cured for 40 seconds.
Self-cure auto-polymerizing acrylic resin was poured into cylindrical moulds and the
specimens were aligned vertically along their long axis. The pull out bond strength of
posts was tested with the help of a universal testing machine at a rate of
0.5mm/minute until the post separated from the root.
The obtained data was subjected to one way ANOVA test and Independent t test.
RESULTS
The mean force required for debonding the posts and standard deviations obtained
are shown in Table 1. Highest mean value of pull out bond strength was observed for
sub-group A1 (312.20 N).Lowest mean value of pull out bond strength was observed
for sub-group A2 (133.47).
The one way ANOVA test showed that the type of chelator used for post space
conditioning significantly influenced the bond strength of glass fibre posts (p=.000).
In addition, the type of luting cement used also demonstrated a statistically
significant difference in the post retention (p=.000) (Table 2).

The independent t test showed a statistically significant difference in bond strength

values of all the sub-groups (p=.000) except between sub-group A2 and B2 (p=.565).
Moreover, the independent t test also confirmed that 17% EDTA exhibited
significantly higher bond strength values compared to 0.2% Chitosan solution. (Table
2)
DISCUSSION
When failures of bonded fibre post and core were assessed, two recent reviews
concluded that a common mode of clinical failure for these restorations was loss of
retention. Hence, there is a definite need for materials and methods that improve the
retention of these increasingly popular restorations. 18,21
One commonly proposed method of improving the retention of fibre posts is by
removal of smear layer by conditioning the post space before application of luting
cement. Application of 17% EDTA as a final irrigating solution, promotes adequate
cleaning of the root canals, consequently improving the penetration of luting agents
and better contact between the dentin walls and the resin material (Arslan H et al). 22
In the present study, fibre posts bonded in EDTA conditioned post spaces showed
higher pull out bond strength values.
17% EDTA facilitates the bonding of fibre posts and improves retention by removing
the smear layer and debris on the dentin surface (Xia Y and Cheng X).23 Post space
conditioned with 17% EDTA produces higher bond strength and more distinct resin
tag formation as compared to NaOCl (Alkhudhairy F et al). 24 EDTA conditioning
provides thinner hybrid layer with no denaturation of collagen (Takarada K).25

No study was found in the literature to validate the effect of 0.2% Chitosan solution
as a post space conditioner on the pull-out bond strength of glass fibre posts. The
chelating effect of chitosan for endodontic applications had not been widely studied;
however adsorption, ionic exchange and chelation are probably the mechanisms
responsible for the formation of complexes between chitosan and metal ions. 26

Chelating and demineralizing solutions act on the hydroxyapatite calcium matrix of

the dentine, with subsequent collagen exposure and reduction of microhardness.
The solution with the ability to remove the highest concentration of calcium ions
presents a higher demineralizing capacity and a higher cleaning potential. 27 Atomic
absorption spectrophotometry with flame analysis of 0.2% Chitosan revealed a
calcium ion concentration of (104.13 19.23), compared with 15% EDTA (121.80
5.13) signifying greater smear layer removal with EDTA (Silva PV et al). 28 This can
be one of the possible reasons for poor performance of Chitosan.
Another possible reason for lack of performance of 0.2% Chitosan could be the
formation of insoluble complexes with calcium ions in the root dentin. As Chitosan is
insoluble in water, traces of Chitosan and calcium complex can still be present in the
post space even after a final irrigation with distilled water. However, this is just a
hypothesis and further SEM evaluations and research are required for validation.
Another variable tested in the present study was the effect of luting agent on the pull
out bond strength of fibre post in the conditioned post space. In the present study
RelyX U200 showed higher bond strength values in both the Chitosan and EDTA
conditioned post spaces. These results corroborate with the findings of other similar
studies in literature.29,30
RelyX U200 relies on phosphoric acid methacrylates, which demineralize and
infiltrate the tooth substrate, resulting in micromechanical retention, and secondary
chemical reactions with hydroxyapatite. It contains a new rheology modifier reducing
the viscosity of the material. This may have contributed significantly to the general
superior bonding performance in comparison to SmartCem2. 31

SmartCem2 is composed polymerizable resins that provide structural reinforcement

of the resin cement, as well as providing strong crosslinking of the polymer network
upon polymerization. The adhesion promoter, PENTA, has been demonstrated to
interact directly with the calcium in tooth structure, resulting in strong covalent
bonding to the tooth surface. 32 Some disadvantages of SmartCem 2 have been cited
in literature- Less flexural modulus than other self-adhesive resin cements, flexural
modulus reduced by simulated environmental storage conditions and no long-term
data on performance and reliability of this self-adhesive resin luting system. 33
PH also plays a significant role in the bond strength of luting agents. Low pH values
for SmartCem2 and RelyX U200 a few seconds after manipulation have been
reported. However, after 48 hours, only RelyX U200 presents a neutral pH (pH=7.0)
in contrast to SmartCem2 (pH=4.0). Even though an initial low pH is important for
etching of enamel and dentin, if a low pH is maintained for a long time, it can
adversely influence the adhesion of the mixed cement to dentin (Han et al). 34
In the light of present discussion and within the limitation of the present study it can
be concluded that 17% EDTA conditioning of post space proved to be beneficial for
improving the pull-out bond strength of glass fibre posts as compared to 0.2%
Chitosan. When used in combination with RelyX U200 self-adhesive resin cement,
17% EDTA provided best results for retention of glass fibre posts. The results of the
present study need to be verified and validated with similar or different variables in
materials and methodology.
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Table 1: Mean and Standard deviation Values (N) in Different Groups

SUB-GROUPS

A2
A1

MEAN
STANDARD

EDTA

+ B1

B2

EDTA + RELYX SMARTCEM2

CHITOSAN

U200
312.20
36.356

RELYX U200
193.00
46.543

133.47
20.392

+ CHITOSAN
SMARTCEM2
137.80
20.355

DEVIATION

Table

2:

Comparison

Between

Mean

Values

of

Different

Sub-Groups

(Independent 't' Test)

Pairs of
t - test

p Value

16.607

.000**

7.817

.000**

16.211

.000**

-4.538

.000**

Group
Group
A1 & A2
Group
A1 & B1
Group
A1 & B2
Group
A2 & B1
Group

-0.582

A2 & B2
Group
B1 & B2
** Significant values

0.565
4.208

.000**