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Int J Oral-M ed Sci 5(1):31-36, 2006

Original Article

Tensile Bond Strength of 4-META/MMA-TBB Resin to Saliva Contaminated Teeth
Using Self-Etching Primer
Somsak Sirirungrojying, Tohru Hayakawa, Daijiro Meguro, and Kazutaka Kasai
Faculty of Dentistry, Thammasat University, Klong Luang, Pathum Thani 12121, Thailand
Departments of Dental Biomaterials, Orthodontics,and Research Institute of Oral Science,Nihon University School
of Dentistry at M atsudo, M atsudo, Chiba 271-8587, Japan
Correspondence to :
Somsak Sirirungrojying

Keywords :
Tensile bond strength, 4-M ETA/
M M A-TBB resin, M egabond selfetching primer,phosphoric acid etching, saliva contamination

The aim of this study was to evaluate the tensile bond strength of 4META/MMA-TBB resin to enamel using a self-etching primer with
saliva contamination. The polished human molar surface was etched
with phosphoric acid or Megabond self-etching primer with or without
saliva contamination,then bonded with Superbond C&B resin cement.
The tensile bond strengths were measured after immersion in water at
C for 24 hours.Without saliva contamination,there was not significantly different between phosphoric acid etching and Megabond (P>
0.05). When the surfaces were saliva contaminated, using phosphoric
acid etching showed decreasing in bond strength significantly (P<
0.05). Comparing to using Megabond, the bond strength decreased
nonsignificantly (P>0.05). The SEM showed the difference of enamel
surface after phosphoric acid etching and Megabond. In conclusion,
comparing the tensile bond strength, Megabond is a better candidate
for etching enamel than phosphoric acid when clinical used.

Superbond C&B (Sunmedical Co. Ltd., Shiga,
Japan) is a unique adhesive resin cements and has
been widely used for bonding orthodontic brackets to
enamel in direct bonding technique. It is methyl
methacrylate (MMA)initiated by partly oxidized tri
-n-butyl borane(TBB)in the presence of polymethyl

reduces of clinical steps and operation time compared to phosphoric acid etching.In case of orthodontic
treatment, the use of phosphoric acid etchings show
the association with enamel loss and a risk ofenamel
cracks and scratches after debonding brackets (6,7).
In addition, phosphoric acid etching has also been

blamed for decalcification and the development of
methacrylate (PMMA) and contains the adhesive white spot lesions around bonded orthodontic applimonomer, 4-methacryloxyethyl trimellitate anhy- ances (8).Thus,some self-etching primer systems are
dride (4 META),dissolved in MMA (1-3).This resin now introduced for bonding orthodontic bracket to
is known as 4-META/MMA-TBB resin,and is also enamel (9, 10).
known as C&B Metabond (Parkell Inc,Farmingdale,
During clinical procedures, it is difficult to comNY)in North America.The bonding to enamel with
Superbond is achieved by 65% by weight phosphoric

plete the prevention of saliva and blood contamination. Reports show that using phosphoric acid etch-

acid etching.
Instead of phosphoric acid, self-etching primer
have become widely used in composite resin restoration (4, 5). Self-etching primers function as both an

ings, contaminations can decrease the bond strength
when bonding with resins (11-13). Compare to using
self-etching primers, contaminations did not affect
the shear bond strength (9, 10).
Previously, we demonstrated that the use of self-

etching agent and a primer. Water rinsing is not
required. Thus, the use of self-etching primer

etching primer with Superbond C&B produced com-

Int J Oral-M ed Sci 5(1):31-36, 2006

patible bond strength more than with phosphoric
acid etching,with less enamel fracture after debonding the orthodontic bracket from enamel. Saliva
contamination significantly decreased the shear
bond strength with phosphoric acid etching, but did
not cause any decrease of bond strength with selfetching primer treatment (9).
The shear or tensile bond strength evaluation was
always considered in traditional bond strength
studies. Each bond strength is different in some
circumstances, such as the adhesive thickness of the
bonding cement (14), bonding durability (15). We
already evaluated the effectiveness of the use of self
-etching primer with Superbond C&B by measuring
the shear bond strength as described above (9).
Kitayama et al (15). compared the tensile and shear
bond strength of resin-reinforce glass ionomer
cement to glazed porcelain, and they reported that
shear bond strength was higher approximately three
to four times more than tensile bond strengths.Smith
and Reynolds suggested that tensile bond strength of
approximately 5-7 MPa was adequate for clinical
success (16).The tensile bond strength of Superbond
C&B resin to bovine enamel using self-etching
primer were already studied (17, 18), but not to
human enamel. Because it is important to evaluate
the efficacy of the use of self-etching primer with
Superbond C&B in orthodontic treatments,the evaluation using tensile bond strength will be useful.
The present study aimed at comparing the tensile
bond strength to enamel between self-etching primer
and phosphoric acid with and without saliva contam-

Fig.1. Schematic drawing of the specimen for tensile bond
strength measurement.

cups for 10 seconds.In all protocols,Superbond C&B
resin cement was used for bonding. As self-etching
primer, Megabond (Kuraray Medical Inc., Tokyo,
Japan)was used.Megabond is composed of 10-methacryloxydecyl dihydrogen phosphate (M DP), 2hydroxyethyl methacrylate,a polyfunctional dimethacrylates.This self-etching primer is a component of
the Clearfil Megabond System (Kuraray M edical
Inc.,), as known as Clearfil SE Bond outside Japan.
Group 1 : Phosphoric acid etching. The teeth were
etched with 65% phosphoric acid gel for 30 seconds,
washed for 20 seconds, and air-dried.
Group 2 : Phosphoric acid before contamination.

ination when bonding with Superbond C&B. The

The teeth were etched with 65% phosphoric acid gel

obtained tensile bond strengths were evaluated by
comparing with previous shear bond strength.

for 30 seconds. After rinsing and drying, the etched
surface was contaminated with 20μl of human fresh
whole saliva.The contaminant fluids were left on the
surface 30 seconds to simulate extremely severe

Tensile Bond Strength Measurement
clinical conditions.Then blowing off the saliva for 5
Fig.1 shows the schematic drawing of the speci- seconds.
men for tensile bond strength measurement. A total
Group 3 : Self-etching primer. The teeth were
of 80 human molar teeth were used in this study. etched with Megabond Self-etching primer for 30
They were randomly allocated into 4 groups of 20
teeth each. The buccal surface were cleansed and
then polished with pumice and rubber prophylactic

seconds. The excessive solution was evaporated
using compressed air.
Group 4 : Self-etching primer before contamina-

Int J Oral-M ed Sci 5(1):31-36, 2006

tion. The teeth were etched with Megabond selfetching primer for 30 seconds.The excessive solution
was evaporated using compressed air.Then,the self
-etching primed enamel was contaminated with 20μl
of human fresh whole saliva.The contaminant fluids
were left on the surface for 30 seconds to simulate
extremely severe clinical conditions.
The area of adhesion was standardized by using a
piece of 300μm-thick masking tape with a hole
measuring 4.0 mm. in diameter.

The results of tensile bond strength of phosphoric
acid etching and self-etching primer with and without saliva contamination are presented in Fig.2.
Two-way ANOVA showed significant differences in
bond strength between phosphoric acid etching and
self-etching primer treatment (P<0.05), and also
showed significant differences in bond strength
between with and without saliva contamination (P<
0.05). Two-way interaction was found for the types
of pretreatment ; etching and self-etching priming
and with and without saliva contamination (P<0.05).

The Superbond C&B resin cement was prepared
by adding the catalyst (partially oxidized TBB) to
Without saliva contamination,there was no signifthe monomer liquid to become active monomer liquid.The polymer powder and active monomer liquid icantly difference in tensile bond strength between
were mixed and applied to bond a sandblasted stain- phosphoric acid etching and self-etching primer (P>
less steel rod to the enamel using brush dip technique. 0.05).In contrast,when teeth were contaminated with
After curing the resin, all specimens were stored in saliva, self-etching primer produced showed signifiwater at 37°
C for 24 hours. Then, the bond strength
was measured using computer-controlled Instron
testing machine (TG-5kN),Minebea,Tokyo,Japan).
The comparison in mean tensile bond strength
between 2 groups was analyzed by two-way analysis
of variance (ANOVA)and Fishers test for multiple
analysis. The level of significance was predetermined at P<0.05.
FE -SEM observation
The human enamel surfaces were cleansed and
then polished with pumice and rubber prophylactic
cups as described above. Two specimens were prepared. One was etched with phosphoric acid for 30
seconds and washed for 20 seconds. Another specimen was treated with Megabond self-etching primer

cantly higher tensile bond strength than phosphoric
acid etching (P<0.05). When used with self-etching
primer, there was no significant difference between
with and without saliva contamination (P>0.05).
Phosphoric acid etching showed significant decrease
in tensile bond strength after saliva contamination
(P<0.05). Macroscopic observation of debonded
specimens showed an adhesive-resin enamel failure
in all groups.No enamel fracture was observed after

for 30 seconds, and excess solution was evaporated
using compressed air. The primed enamel surface
was rinsed with acetone for 30 seconds to remove the
organic components of the self-etching primer.Both
etched and self-etching primed specimens were dehydrated through a graded series of ethanol,dried in a
critical apparatus, and ion-coated with platinum.
The surface appearances of etched and primed
tooth specimens were observed using a field-emistween stainless steel rod and
sion scanning electron microscope (FE-SEM ; JSM - Fig.2. Tensile bond strength be/
6340F, Tokyo, Japan).

human enamel when used with 4 META MMA TBB resin.
, : significant difference

Int J Oral-M ed Sci 5(1):31-36, 2006

Fig.3. FE-SEM micrographs of enamel surfaces etched with phosphoric acid (3a)or treated with self-etching primer (3b).

Fig.3 showed the FE-SEM micrographs of human
enamel surfaces that have been etched with phosphoric acid (Fig.3a) and treated with Megabond
primer (Fig.3b).Phosphoric acid etching produced a
finely roughened enamel surface with random
arrangement of enamel crystals. Dissolution of both
enamel prisms and peripheries was observed. The
appearances of enamel surface after Megabond
primer treatment was different from that observed
after phosphoric acid etching (Fig.3b).There was no
distinct dissolution pattern and the enamel surface
appeared almost flat.No enamel crystals were observed.

In the present study,we demonstrated the efficacy
of self-etching primer with the use of Superbond C&
B when teeth were contaminated with saliva by
measuring the tensile bond strength.
When tooth was not contaminated with saliva, no
significant difference existed in the tensile bond
between phosphoric acid and self-etching primer. It
is generally recognized that mechanical retention on
roughened enamel contributes to the adhesion of
dental resins to enamel (19). However, the appearance of self-etching primed enamel surface was

finding suggest that the main adhesion contributor
comes not from the mechanical retention obtained by
macro-resin tags but from the formation of microresin tags (18).
The present study found that saliva contamination
did not decrease the tensile bond strength to selfetching primed enamel. It is hypothesized as following although the detailed mechanism is unknown.
Because the self-etching primer treatment did not
produce distinct dissolution pattern on enamel, the
saliva cannot penetrate into the primed enamel and
the contaminated saliva on self-etching primed
enamel is too thin. Thus,adhesive resin can bond to
saliva contaminated enamel.
In the comparison between tensile and shear bond
strength, the tensile bond strength obtained in the
present study was approximately one third of previous shear bond strength (15-21 MPa)(9). Thomas et
al. evaluated the tensile and shear stressed in orthodontic attachment adhesive layer with 3D finite
element analysis (20). They concluded that a typical
tensile load induces predominantly tensile stresses in
the cement interfaces and that the test is relatively
insensitive to minor misalignments errors. In contrast, the shear load produces both tensile stressed
and compressive stressed in the cement interface that
are ofcomparable magnitude or greater as compared

completely different from that etched by phosphoric
acid : there was no distinct dissolution and no rough- to the shear stress. This is the one of the reason for
ening of self-etching primed enamel surface. These the decrease of tensile bond strength compared with

Int J Oral-M ed Sci 5(1):31-36, 2006

shear bond strength, although the detailed reason is
not clear.
At any event, present tensile bond strength is
clinical acceptable value for bonding orthodontic
bracket even if teeth is contaminated with saliva,
according to the suggestion by Smith and Reynolds
(16).In addition,self-etching primer treatment has a
benefit for less damage for enamel dissolution. The
use of Megabond primer with Superbond C&B for
bonding orthodontic bracket to enamel may have a
lower risk of enamel fracture at the time of debonding.
The lower value of tensile bond strength compared
with shear bond strength also suggested that
removal of bonded orthodontic bracket by tensile
force is more desirable than shearing force in orthodontic clicnis. In the clinical situation, the purpose
is not to obtain the highest possible bond strength,
but to obtain adequate bond strength for orthodontic
treatment, and safe debonding without any damage
in enamel is very important.
In conclusion, the present study revealed the usefulness of Megabond self-etching primer with Superbond C&B resin cement by measuring the tensile
bond strength besides the measurement ofshear bond

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