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Incompatibility of Oxalate Desensitizers with

Acidic, Fluoride-containing Total-etch
Adhesives

Article in Journal of Dental Research · August 2005

DOI: 10.1177/154405910508400809 · Source: PubMed

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 RESEARCH REPORTS
Biomaterials & Bioengineering
C.K.Y. Yiu1, N.M. King1, B.I. Suh2,
L.J. Sharp2, R.M. Carvalho3,
D.H. Pashley4, and F.R. Tay1*
1 Paediatric Dentistry and Orthodontics, Faculty of
Dentistry, The University of Hong Kong, 34 Hospital Road,
Hong Kong SAR, China; 2Bisco Inc., Schaumburg, IL,
USA; 3Department of Operative Dentistry, Endodontics and
Dental Materials, Bauru School of Dentistry, University of
São Paulo, Bauru, SP, Brazil; and 4Department of Oral
Biology and Maxillofacial Pathology, School of Dentistry,
Medical College of Georgia, Augusta, GA, USA;
*corresponding author, kfctay@netvigator.com
J Dent Res 84(8):730-735, 2005
ABSTRACT
The use of oxalate desensitizers on acid-etched
dentin prior to adhesive application can result in
subsurface tubular occlusion by calcium oxalate
crystals. However, the solubility of calcium
oxalate increases in acidic solution. We
hypothesized that total-etch adhesives can,
depending upon their pH, interact with oxalate-
desensitizer-treated dentin in an adverse manner.
Acid-etched human dentin treated with 2 oxalate
desensitizers (BisBlock and Super Seal) was
bonded with 4 simplified total-etch adhesives:
One-Step (OS), Single Bond (SB), OptiBond Solo
Plus (OB), and Prime&Bond NT (PB).
Composite-dentin beams were examined by SEM
and TEM, both of which revealed numerous
spherical globules on OB- and PB-bonded,
desensitizer-treated dentin, but not in OS or SB
samples. Bond strengths produced by OB and PB
were significantly lower in oxalate-treated
specimens than those produced by OS or SB.
These surface globules may have interfered with
hybridization of demineralized dentin with OB
and PB resins and caused compromised bond
strengths.
KEY WORDS: oxalate desensitizer, acid-etch,
single-bottle adhesives, pH, fluoride.
Received August 27, 2004; Last revision May 12, 2005;
Accepted May 13, 2005
A supplemental appendix to this article is published
electronically only at http://www.dentalresearch.org.
730
Incompatibility of Oxalate
Desensitizers with Acidic,
Fluoride-containing
Total-etch Adhesives
INTRODUCTION
P2001;ost-operative sensitivity is frequently encountered with the use of
adhesives that require the acid-etching of vital dentin (Akpata and Sadiq,
Unemori et al., 2001). The application of these total-etch adhesives
can be technique-sensitive, since wet bonding is required for full expansion
and optimal hybridization of the demineralized collagen matrix (Gwinnett,
1992; Kanca, 1992). The difficulty in bonding is further complicated by the
intrinsic wetness of vital deep dentin after removal of the smear layer
(Itthagarun and Tay, 2000), and the increased permeability associated with
the simplified version of these adhesives (Tay et al., 2003a). Incomplete
sealing and continuous transudation of dentinal fluid through open dentinal
tubules before polymerization of the adhesive may result in entrapment of
water-filled blisters along the adhesive interface (Tay et al., 1996).
Compression of these blisters during mastication may cause, within the
dentinal tubules (Brännström and Johnson, 1970), rapid fluid movement that
activates the intradental A␦ nerve fibers (Närhi et al., 1994), which results
in post-operative sensitivity.
One way of relieving post-operative sensitivity clinically is the
adjunctive use of oxalate desensitizers on acid-etched dentin prior to
adhesive application (Pashley et al., 2001; Tay et al., 2003b). Depletion of
calcium ions from the surface dentin forces the oxalate ions to diffuse
further down into the dentinal tubule, until calcium ions are encountered for
reaction. The calcium oxalate crystals that are formed result in subsurface
tubular occlusion and reduction in the hydraulic conductance of dentin.
However, the solubility of calcium oxalate is affected by pH, since the anion
is the conjugate base of a weak acid (Kotz and Treichel, 1999). Preliminary
screening of the compatibility of oxalate desensitizers with total-etch
adhesive systems revealed complete compatibility with One-Step (Bisco)
and Single Bond (3M ESPE) and poor compatibility with Prime&Bond NT
(Dentsply) and OptiBond Solo Plus (Kerr). This led to a more detailed
investigation seeking the reasons for compatibility vs. incompatibility. The
purpose of this study was to determine if the acidity of total-etch adhesives
may influence their bonding to oxalate-desensitizer-treated acid-etched
dentin.
Thus, the objectives of this study were: (1) to compare the microtensile
bond strengths of 4 single-bottle total-etch adhesives of different acidities to
oxalate-desensitizer-treated acid-etched dentin; and (2) to examine, with the
use of scanning and transmission electron microscopy, the ultrastructure of
the bonded interface. The null hypothesis tested was that there is no
difference in the bonding of single-bottle total-etch adhesives of different
acidities to oxalate-desensitizer-treated acid-etched dentin.
J Dent Res 84(8) 2005 Incompatibility of Oxalate Desensitizers 731

MATERIALS & METHODS
Eighty-four non-carious human third molars, that were stored in a
0.5% chloramine T solution at 4°C, were used within 1 mo
following extraction. The teeth were collected after the patients'
informed consent had been obtained under a protocol approved by
the Institutional Review Board of the Medical College of Georgia,
Augusta, USA. The occlusal enamel was removed with the use of a
slow-speed saw with a diamond-impregnated disk (Isomet, Buehler
Ltd., Lake Bluff, IL, USA) under water cooling. A 180-grit silicon
carbide paper was used under running water to create a clinically
relevant smear layer on the dentin surface.
Experimental Design
Four single-bottle total-etch adhesives and 2 oxalate desensitizers
were investigated. The adhesives were: One-Step (OS; Bisco Inc.,
Schaumburg, IL, USA), Single Bond (SB; 3M ESPE, St. Paul,
MN, USA), OptiBond Solo Plus (OB; Kerr Co., Orange, CA,
USA), and Prime&Bond NT (PB; Dentsply De Trey, Konstanz,
Germany). The oxalate desensitizers were: BisBlock (BB; Bisco
Inc.) and Super Seal (SS, Phoenix Dental Inc., Fenton, MI, USA).
Each adhesive was divided into 3 experimental groups with 7 teeth
each. Five restored teeth were used for microtensile bond strength
evaluation and 2 teeth for ultrastructural examination.
␮TBS)
Microtensile Bond Strength (␮
Bonding was performed on the occlusal surfaces of deep, coronal
dentin. The 3 experimental groups were:
Group 1: The surface to be bonded was etched with a 32%
phosphoric acid gel (Uni-Etch, Bisco Inc.) for 15 sec
and rinsed with water for 20 sec before bonding
occurred.
Group 2: After the surface was acid-etched, BisBlock was
applied with a rubbing motion for 30 sec and rinsed
with water for 60 sec before bonding occurred.
Group 3: After the surface was acid-etched, Super Seal was
applied with a rubbing motion for 30 sec and rinsed
with water for 60 sec before bonding occurred.
The treated teeth were bonded according to the
manufacturers' instructions. Bonded surfaces were air-dried and
light-cured for 10 sec. Composite build-ups were performed with
the use of a light-cured composite (Z250, 3M ESPE) in 5 1-mm
increments and individually light-cured for 40 sec. The teeth were
stored in distilled water at 37°C for 24 hrs. Bonded teeth were
then sectioned occluso-gingivally into 0.9 x 0.9-mm composite-
dentin beams (Shono et al., 1999). Eight beams were retrieved
from the 2 widest slabs of each tooth. Five teeth from each group
yielded 40 beams for bond strength evaluation. Specimens were
stressed to failure under tension in a Bencor Multi-T device
(Danville Engineering, San Ramon, CA, USA) with the use of a
universal testing machine, Model 4440 (Instron, Inc., Canton,
MA, USA), at a crosshead speed of 1 mm/min. Beams with
premature bond failure were assigned a null bond strength value
and were included in the compilation of the mean bond strength.
The data collected were analyzed with SigmaStat Version 2.03
(SPSS, Chicago, IL, USA). Since the ␮ TBS data were not
normally distributed (Kolmogorov-Smirnof test), the data were
analyzed by Kruskal-Wallis one-way ANOVA on ranks and
Dunn's multiple-comparison tests, with statistical significance set
at ␣ = 0.05.
Scanning Electron Microscopy
Four representative fractured beams from each group with ␮TBS
close to the mean bond strength of that group were selected for
fractographic analysis by scanning electron microscopy (SEM).
The dentin sides of the fractured specimens were air-dried, coated
with gold/palladium, and examined with a SEM (Cambridge
Stereoscan 440, Cambridge, UK), operating at 10-20 kV.
Transmission Electron Microscopy
Two teeth from each group were acid-etched and similarly treated
with the oxalate desensitizers in the manner as previously
described. The teeth were sectioned into 0.9-mm slabs. The 2
widest slabs were coated with 2 layers of nail varnish applied 1
mm from the bonded interfaces. They were immersed in a 50 wt%
ammoniacal silver nitrate solution for 24 hrs, according to the
silver impregnation protocol reported by Tay et al. (2002). After
reduction of the diamine silver ions, the silver-impregnated slabs
were processed for transmission electron microscopy (TEM)
without further demineralization, and were examined, unstained,
by TEM (Philips EM208S, Philips, Eindhoven, The Netherlands)
at 80 kV.
Measurement of pH and F Concentration of Adhesives
Water-free adhesives that are dissolved in polar solvents do not
usually dissociate into ionic species. To circumvent this problem,
we dispensed 2-mL specimens of each adhesive into clean glass
vials containing 3 mL of 70% ethanol and 30% distilled water. The
pH values of the 4 adhesive solutions were measured at ambient
temperature (22-25°C) by means of a digital pH meter (Model 501,
Orion Research, Inc., Beverly, MA, USA). Three readings were
taken for each adhesive, and the mean pH value was calculated for
each adhesive.
Similarly to the pH measurement, a 2-mL specimen of each
simplified-step adhesive was dispensed into a clean glass vial
containing 3 mL of 70% ethanol and 30% distilled water. The

Table. pH Values and F Concentrations of the 4 Total-etch, Two-step Adhesives and Their Microtensile Bond Strengths after Bonding to Oxalate-
desensitizer-treated Acid-etched Dentin

Microtensile Bond Strength (MPa)1

F Concentration Control
Adhesives pH (ppm F) (adhesive only, no desensitizer) BisBlock (BB) plus Adhesive Super Seal (SS) plus Adhesive

One-Step (OS) 4.60 70 48.7 (4.2)a [0/40] 43.4 ( 4.8)a [ 0/40] 47.1 (4.8)a [ 0/40]
Single Bond (SB) 3.60 130 47.4 (4.2)a [0/40] 39.6 ( 8.1)a [ 0/40] 40.9 (6.6)a [ 0/40]
OptiBond Solo Plus (OB)2 2.81 4527 49.2 (7.3)a [0/40] 12.6 ( 8.6)b [ 8/40] 16.8 (6.8)b [ 5/40]
Prime&Bond NT (PB)2 2.68 3641 51.8 (4.5)a [0/40] 6.9 (10.6)b [12/40] 5.1 (9.0)b [14/40]

1 Values are means ± standard deviation [N = 40]. Groups identified with the same superscripts are not significantly different (p > 0.05).
2 Beams with premature failure during specimen preparation were included as null bond strengths in the calculation of mean bond strength.
732 Yiu et al. J Dent Res 84(8) 2005

Fluoride Analysis
Ion-specific fluoride analysis of the 4
adhesive systems revealed relatively
low levels in OS and SB (70 and 130
ppm, Table), compared with very high
levels in OB and PB (4527 and 3641
ppm, Table), respectively.
TEM Results
Bonded interfaces from PB-SS speci-
mens revealed extensive nanoleakage
of silver within the hybrid layer, and
electronlucent spherical globules with
silver deposits were observed in the
adhesive layer. Discontinuous
electronlucent spaces could be
identified along the adhesive-dentin
interface (Fig. 2A). Nanoleakage was
also observed within the entire hybrid
layer from OB-BB (Fig. 2B). The
dentinal tubules were filled with silver
deposits, with no subsurface oxalate
crystals identified. Discontinuous
Figure 1. SEM micrographs of the dentin side of a fractured beam following application of single-
bottle total-etch adhesives to oxalate-desensitizer-treated acid-etched dentin. (A) Spherical globules spaces with scalloped margins were
(arrowheads) with sizes ranging from 2 to 4 ␮m were preferentially found at the orifices of the found between the hybrid and
dentinal tubules in the PB-SS subgroup. Clusters of smaller globules (arrow) were found between the adhesive layers in OB-BB. No major
larger globules. Patent dentinal tubules (pointer) were frequently observed. (B) Spherical globules differences could be recognized
(pointers) up to 12 ␮m were also observed in the adhesive layer of the PB-BB subgroup. (C) The
dentin side of the OB-BB subgroup was covered with a continuous layer of spherical globules with between the 2 oxalate desensitizers
sizes ranging from 0.5 to 3 ␮m. Patent dentinal tubules (arrowheads) were evident from the dentin after the application of OB and PB. In
(D) below. (D) No spherical globules could be found on the dentin surface of the SB-SS subgroup. contrast to OB and PB, isolated silver
Numerous fractured resin tags (arrowheads) could be seen at the base of the hybrid layer (H). deposits were found in only some
areas of the hybrid layer of SB-SS
(Fig. 2C) and OS-BB (Fig. 2D).

solution was buffered with TISAB III (Orion Research Inc.). The
fluoride concentrations were determined at ambient temperature by
an ion-selective electrode (Cat. No. 96, Orion Research Inc.).
RESULTS
Microtensile Bond Strength
The ␮TBS of the 4 adhesives, and their measured pH values
and F concentrations are summarized in the Table. Both OB
and PB showed significant reduction in ␮TBS when applied to
oxalate-treated acid-etched dentin (p < 0.05). In contrast, SB
and OS showed no significant differences in bond strength
when applied to oxalate-treated and untreated acid-etched
dentin (p > 0.05). No statistically significant difference was
noted between BisBlock and Super Seal when used with the 4
adhesives.
SEM Results
Adhesive failure occurred predominantly along the adhesive-
dentin interface in PB-SS (Fig. 1A). The dentin surfaces were
characterized by spherical globules (diameter, 2-4 ␮m) located
preferentially at the orifices of the dentinal tubules. Spherical
globules could also be seen in the voids of the adhesive layers
of PB-BB (Fig. 1B). Similarly to PB, numerous spherical
globules were evident on the fractured dentin surfaces of OB-
BB (Fig. 1C). In contrast, the failure mode of the SB and OS-
oxalate subgroups was predominantly "mixed", and no
spherical globules were seen (Fig. 1D).
DISCUSSION
The application of oxalate desensitizers to acid-etched dentin
prior to adhesive application represents one way of avoiding
post-operative sensitivity, since this clinical complication is
highly product-related. Better sealing ability of conventional
three-step total-etch and two-step self-etch adhesives (De
Munck et al., 2005; Frankenberger and Tay, 2005) may
similarly block the effects of hydraulic pressure and reduce
post-operative sensitivity. The results of this study showed that
effective bonding to the desensitizer-treated acid-etched dentin
is adhesive-specific. Since both the microtensile bond strengths
and ultrastructural features of the simplified total-etch
adhesives were different when bonded to oxalate-desensitizer-
treated acid-etched dentin, we have to reject the null hypothesis
tested.
The bond strengths of OS and SB were not compromised
with the adjunctive use of the oxalate desensitizers. Optimal
resin infiltration and hybrid layer formation occurred in the
presence of bi-pyramidal calcium oxalate dihydrate crystals in
the dentinal tubules. These crystals can be seen more clearly in
cryofractured specimens (Fig. 3). In contrast, significantly
lower bond strengths were observed in OB and PB when
applied to oxalate-desensitizer-treated dentin, that could be
attributed to the presence of spherical globules along the
adhesive-dentin interface. These spherical globules closely
resemble the loosely bound spherical calcium fluoride (CaF2)-
like material formed on enamel (Dijkman et al., 1983; Nelson
J Dent Res 84(8) 2005 Incompatibility of Oxalate Desensitizers 733

et al., 1983, 1984) and demineralized

dentin surfaces (Itota et al., 2002)
following topical fluoride treatment.
These spherical globules were removed
by the KOH extraction method
(Caslavska et al., 1975), confirming
that the globules were KOH-soluble
fluoride (Appendix). Regardless of the
composition of the spherical globules
found on the surfaces of oxalate-
treated specimens bonded with the 2
incompatible adhesive systems (OB
and PB), their presence at the bonded
interface and in the adhesive layer
could serve as stress-raisers that would
create debonding at lower stresses than
would occur in their absence. TEM
examination of the bonded interface
also revealed discontinuous
electronlucent spaces with distinct
"scalloped" margins. These were not
true gaps along the adhesive-dentin
interfaces, since they were not
infiltrated by silver deposits. The
"scalloped" margins correlated nicely
with the shapes of spherical globules.
Variability was seen in size and
distribution densities of these globular
structures following the application of
PB and OB to oxalate-desensitizer-
treated dentin. This could be due to the
differences in concentration of Figure 2. Unstained, undemineralized TEM micrographs of oxalate-desensitizer-treated acid-etched
fluoride, pH values of PB and OB, and dentin specimens that were bonded with single-bottle total-etch adhesives. The bonded specimens
the availability of calcium ions on the were immersed in an ammoniacal silver nitrate tracer solution before laboratory dehydration and
dentin surface (Arends et al., 1988; epoxy resin embedding. U: undemineralized dentin. (A) A specimen from the PB-SS subgroup,
showing extensive nanoleakage (open arrowheads) in the hybrid layer (H) and the dentinal tubule
Saxegaard and Rölla, 1988). Both PB (T). Electronlucent spherical globules (pointer) were depicted in the adhesive layer (A). Silver
and OB are fluoride-containing deposits were occasionally seen within the spherical globules. Discontinuous electronlucent structures
adhesives; it is reasonable to assume with a scalloped margin could be identified along the adhesive-hybrid layer interface (open arrow).
that the free fluoride ions from the Electronlucent crystals, probably representing the calcium oxalate crystals (arrow), were also seen in
adhesives may interact with calcium the dentinal tubules at a position that was 8-10 ␮m from the dentin surface. (B) A specimen from the
OB-BB subgroup, showing fairly extensive nanoleakage (arrowhead) within the hybrid layer (H).
and phosphate ions on dentin surfaces Discontinuous electronlucent deposits, with scalloped margins resembling conglomerates of spherical
to precipitate CaF2-like material. The globules (pointer), could be identified along the adhesive-dentin interface. Subsurface electronlucent
greater intensity of fluoride deposition deposits (asterisk) were also observed in the dentinal tubules (T). (C) A high-magnification view of
in OB may be explained by the higher the hybrid layer in the SB-BB subgroup. Only isolated spots of silver grains (arrowhead) were
observed in the hybrid layer (H). No globular structures were identified on the surface of the hybrid
F concentration in OB (4527 ppm) vs. layer. The dentinal tubules (beneath the position of the hybrid layer) were blocked by subsurface
PB (3641 ppm, Table). Conversely, no electronlucent deposits (asterisk). P: polyalkenoic acid copolymer component of the adhesive. (D) A
globular structures were formed high-magnification view of subsurface angular crystalline deposits (asterisk) within the dentinal
following the application of OS and SB tubule (T) in the OS-BB subgroup. No surface globular structures could be identified. Silver deposits
to oxalate-treated dentin, since these (arrowhead) were occasionally observed within the hybrid layer (H). A: adhesive.
adhesives contain minimum amounts
of fluoride (Table). The presence of
spherical globules on the surface of the
desensitizer-treated dentin may hinder
the adhesive infiltration and hybridization of demineralized formation of the spherical globules in OB- and PB-bonded
dentin. This is supported by the TEM results, where extensive specimens, the availability of calcium ions on the dentin
accumulation of silver deposits was observed in the porous surface is also critical. Since the dentin surface was completely
hybrid layers following the application of PB and OB to deprived of calcium phosphate following phosphoric-acid-
oxalate-treated dentin. Similar effects have recently been etching (Van Meerbeek et al., 2003), the calcium ions could
reported following the application of hydrofluoric acid gel to have been derived from the dissolution of calcium oxalate
acid-etched dentin (Szep et al., 2000; Pioch et al., 2003). crystals in the dentinal tubules. The solubility of calcium
Although the presence of fluoride ion is necessary for oxalate (CaC2O4) is affected by pH, since the anion is the
734
Figure 3. SEM micrograph of cryofractured phosphoric-acid-etched
dentin following the application of an oxalate desensitizer. Bi-pyramidal
calcium oxalate crystals (open arrowhead) were identified in the
dentinal tubules, at 8-10 ␮m beneath the dentin surface, where calcium
ions were available from the adjacent mineralized dentin (D). In
contrast, the demineralized collagen matrix (asterisk) was almost
completely devoid of these angular crystals. Since no acidic, fluoride-
containing dentin adhesive was further applied to the desensitizer-
treated dentin, the etched dentin surface was devoid of the spherical
calcium-fluoride-like structures. Only demineralized collagen fibrils
(pointer) were identified from the surface of the acid-etched dentin.
conjugate base of a weak acid. The low pH values of OB and
PB may increase the solubility of calcium oxalates in the
dentinal tubules. According to Le Châtelier's principle
(Silberberg, 2003), as calcium oxalate crystals are exposed to
more H3O+, more calcium oxalate dissolves into calcium and
oxalate ions, to compensate for the depletion of oxalate ions
and maintain the equilibrium constant. This is supported by the
SEM observation of considerably fewer, and smaller, calcium
oxalate crystals in the dentinal tubules following the
application of OB and PB to oxalate-desensitizer-treated
dentin.
In conclusion, the results of the present in vitro study
indicated that the bond strength of simplified total-etch
adhesives to oxalate-desensitizer-treated acid-etched dentin
may be compromised by the acidity and the availability of
fluorides from some total-etch adhesives. In vivo studies are
needed to confirm these in vitro observations. Clinicians
should be aware of the potential drop in bond strength with the
use of PB and OB on oxalate-desensitizer-treated acid-etched
dentin.
ACKNOWLEDGMENTS
This study was based on the work partially performed by
Cynthia Yiu for the fulfillment of the degree of Doctor of
Philosophy, the University of Hong Kong. The authors express
their gratitude to Bill Lee of the Electron Microscopy Unit, the
University of Hong Kong, for technical assistance, and to Jenny
Wang of Bisco Inc. for advice. The products examined in this
study were generously sponsored by the manufacturers. This
study was supported by RCG CERG grant
10204604/07840/08004/324/01, Faculty of Dentistry, The
University of Hong Kong, by grants DE 014911 and DE
015306 from the National Institute of Dental and Craniofacial
Yiu et al. J Dent Res 84(8) 2005
Research, USA (P.I., David Pashley), and by grants 300481/95-
0 and 474226/03-4 from CNPq, Brazil. The authors thank
Frances Chow and Michelle Barnes for secretarial support.
Byoung Suh is President of Bisco, Inc., the company that
manufactures BisBlock, the oxalate desensitizer used in this
study. Louis Sharp is an employee of Bisco, Inc. Drs. Carvalho
and Pashley are the inventors of the patented oxalate
desensitizer used in this study. The other authors have no
financial interest in any of the products.
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