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Margin Integrity of Conservative Composite Restorations

after Resin Infiltration of Demineralized Enamel


Philipp Körnera / Mohamed El Gedailyb / Rengin Attinc / Daniel B. Wiedemeierd / Thomas Attine /
Tobias T. Tauböckf

Purpose: To investigate the influence of pretreating demineralized enamel with a caries infiltrant on the margin in-
tegrity of Class V composite restorations bonded with different adhesives.
Materials and Methods: A total of 60 specimens from bovine incisors were demineralized (21 days, acid buffer, pH
4.95) to create artificial enamel lesions, and circular Class V cavities were prepared. Cavities of half of the speci-
mens were treated with either an unfilled etch-and-rinse adhesive (Syntac Classic; Ivoclar Vivadent), a filled etch-
and-rinse adhesive (Optibond FL; Kerr), or a self-etch adhesive (iBond Self Etch; Heraeus Kulzer) (n = 10 per
group). Demineralized enamel of the other half of the specimens was pretreated with a caries infiltrant (Icon; DMG)
prior to adhesive application. All cavities were restored with a nanofilled composite material and thermocycled
(5000×, 5°C–55°C). Margin integrity was evaluated using scanning electron microscopy, and the percentage of
continuous margin was statistically analyzed (p < 0.05).
Results: The significantly highest margin integrity was observed for Optibond FL, whether or not demineralized
enamel was pretreated with the infiltrant. Pretreatment of demineralized enamel with the infiltrant resulted in a sig-
nificant increase in margin integrity when the unfilled etch-and-rinse adhesive (Syntac Classic) or the self-etch ad-
hesive (iBond Self Etch) was subsequently applied, but showed no significant improvement in combination with the
filled etch-and-rinse adhesive (Optibond FL).
Conclusion: Application of a caries infiltrant can improve margin integrity of composite fillings in demineralized
enamel when used in combination with the examined self-etch and unfilled adhesives.
Keywords: caries infiltrant, margin integrity, demineralized enamel, resin composite

J Adhes Dent 2017; 19: 483–489. Submitted for publication: 13.07.17; accepted for publication: 20.09.17
doi: 10.3290/j.jad.a39280

a Resident, Clinic of Preventive Dentistry, Periodontology and Cariology, Center of


Dental Medicine, University of Zurich, Zurich, Switzerland. Wrote the manuscript.
I n the era of adhesive dentistry, healthy dental tissues can
be conserved through lesion-oriented, minimally invasive
caries treatment. The fundamental prerequisite is the real-
b Master’s Student, Clinic of Preventive Dentistry, Periodontology and Cariology, ization of optimum bond strength on dental hard tissues
Center of Dental Medicine, University of Zurich, Zurich, Switzerland. Per-
formed the experiments in partial fulfillment of requirements for a master’s and a high degree of margin integrity between tooth and
degree, proofread the manuscript. restoration.16 In order to achieve this aim, traditional exca-
c Dentist in Private Practice, Senior Research and Teaching Assistent, Clinic of vation concepts recommend complete removal of softened
Orthodontics and Pediatric Dentistry, Center of Dental Medicine, University of
Zurich, Zurich, Switzerland. Research idea, proofread the manuscript.
dentin and demineralized enamel margins.2,8 Especially in
d
non-cavitated areas of demineralized enamel, this concept
Research Associate in Data Analysis and Statistics, Center of Dental Medi-
cine, University of Zurich, Zurich, Switzerland. Performed statistical evalu- may lead to a disproportionately high loss of dental hard
ation, proofread the manuscript. tissue.23
e Professor and Director, Clinic of Preventive Dentistry, Periodontology and Cari- Infiltration of caries lesions with low viscosity resins is
ology, Center of Dental Medicine, University of Zurich, Zurich, Switzerland.
Research idea, contributed substantially to discussion, proofread the manu-
considered a treatment option for non-cavitated lesions
script. which are not expected to arrest or remineralize.21 This
f Head of Division of Cariology, Clinic of Preventive Dentistry, Periodontology idea seems to be supported by a recent paper, in which
and Cariology, Center of Dental Medicine, University of Zurich, Zurich, Switzer- marginal adaptation of fissure sealants in natural, non-exca-
land. Research idea, hypothesis, experimental design, contributed substan-
tially to discussion and writing the paper, proofread the manuscript. vated occlusal lesions was shown to benefit from resin infil-
trant pretreatment.23 Through low viscosity, low contact
Correspondence: Dr. Philipp Körner, Clinic of Preventive Dentistry, Periodontol- angle to enamel, and high surface tension, caries infiltrants
ogy and Cariology, Center of Dental Medicine, University of Zurich,
Plattenstrasse 11, CH-8032 Zurich, Switzerland. Tel: +41-44-634-3386; have been optimized to penetrate the porous lesion body
e-mail: philipp.koerner@zzm.uzh.ch deeper than conventional adhesives, and can act as a diffu-

Vol 19, No 6, 2017 483


Körner et al

ESPE, St Paul, MN, USA). In order to avoid internal demin-


eralization, the pulp cavum of the specimens was blocked
and sealed with nail polish. The enamel was demineralized
by storing the specimens for 21 days at 37°C in an acid
buffer containing 3 mM CaCl2 × 2 H2O, 3 mM KH2PO4,
6 μM MHDP, 50 mM CH3COOH, KOH (to adjust the pH to
4.95), and distilled water.6 The solution was renewed every
Enamel
day to keep the pH constant. A cross-sectional cut of an
artificially demineralized enamel lesion is illustrated in
Fig 1. After demineralization, standardized Class V cavities
(diameter: 3 mm, depth: 2 mm, bevel edge: 1 mm) were
prepared on the labial surface using spherical-head dia-
Dentin mond burs (D126, Garant; Munich, Germany). The entire
200 μm margin was located in enamel.

Fig 1 Cross-section of an artificially demineralized enamel lesion Infiltration and Bonding Procedure
after 21 days in acid buffer (left) vs no demineralization (right).
The experimental design is illustrated in Fig 2. Demineral-
ized, prepared specimens were randomly assigned to six
groups of ten specimens each. While in groups 1–3 the
sion barrier to prevent acid penetration.28,35 Nevertheless, cavities were solely treated with either an unfilled etch-and-
extensive areas of demineralized enamel might also exhibit rinse adhesive, a filled etch-and-rinse adhesive, or a self-
cavitated defects.22 As caries infiltrants are able to pene- etch adhesive, demineralized enamel in groups 4–6 was
trate most parts of demineralized enamel, but cannot fill pretreated with a caries infiltrant prior to adhesive applica-
the cavitation itself,32 the question arises whether resin tion. Detailed information and composition of the infiltrant
infiltration might be combined with conventional adhesives system and adhesives are given in Table 1.
prior to placement of a composite restoration to enable res- The infiltration and bonding procedure in the different
toration of cavitated and infiltration of demineralized groups was strictly based on the manufacturers’ instruc-
areas.19 tions for use, and was performed as follows:
In this context, the applicability of different adhesives y Group 1: Unfilled etch-and-rinse adhesive (Syntac Clas-
(unfilled etch-and-rinse, filled etch-and-rinse, self-etch) in sic)
combination with a caries infiltrant, and their influence on Enamel and dentin surfaces were etched with 37% phos-
the margin integrity of composite restorations, are of great phoric acid gel (Total Etch; Ivoclar Vivadent, Schaan,
interest. While the filled adhesive Optibond Fl is considered Liechtenstein) for 15 s before rinsing with water for
the gold standard of etch-and-rinse adhesives,39 the un- 30 s. After gently air drying, the adhesive (Syntac Clas-
filled adhesive Syntac Classic and self-etch adhesive iBond sic; Ivoclar Vivadent) consisting of Syntac Primer (15 s),
Self Etch were chosen, as they are frequently used in vari- Syntac Adhesive (10 s) and Heliobond (15 s), was ap-
ous in vitro and in vivo studies and can be regarded as plied and light cured (20 s). Photoactivation was per-
sound representatives of their respective group.4,6,40 The formed using a polywave LED curing unit (Bluephase G2,
distinct adhesives not only differ in filler content and poly- Ivoclar Vivadent) at an irradiance of at least 1100 mW/
merization shrinkage, but also in their viscosity, which cm2. Output irradiance of the curing unit was checked
might have an influence on their penetration into demineral- periodically with a calibrated power meter (FieldMaxII-TO,
ized enamel. Coherent; Santa Clara, CA, USA).
Therefore, the aim of the present study was to evaluate y Group 2: Filled etch-and-rinse adhesive (Optibond FL)
margin integrity of composite restorations in demineralized Prior to application of the filled etch-and-rinse adhesive
enamel after application of three different adhesives with (Optibond FL, Kerr; Orange, CA, USA), enamel and dentin
and without caries infiltrant pretreatment. The null hypoth- surfaces were etched with 37% phosphoric acid gel for
eses were that 1) pretreatment with a caries infiltrant and 15 s and rinsed for another 30 s. After primer application
2) different kinds of adhesives do not affect the margin in- for 15 s and gently air drying for 5 s, the adhesive was ap-
tegrity of composite restorations in demineralized enamel. plied for 15 s, gently air thinned, and light cured for 20 s.
y Group 3: Self-etch adhesive (iBond Self Etch)
Enamel and dentin surfaces were conditioned by apply-
MATERIALS AND METHODS ing the self-etch adhesive (iBond Self Etch, Heraeus Kul-
zer; Hanau, Germany) for 20 s, followed by gentle air dry-
Specimen Preparation and Demineralization ing (5 s) and light curing (20 s).
A total of 60 specimens were prepared from the crowns of y Group 4: Caries infiltrant + unfilled etch-and-rinse adhe-
freshly extracted, undamaged, permanent bovine incisors sive (Syntac Classic)
stored in tap water until use. The cementum layer was en- Demineralized enamel around the circular cavity (bevel
tirely removed using polishing disks (Sof-Lex Pop-on; 3M edge included) was etched with 15% hydrochloric acid

484 The Journal of Adhesive Dentistry


Körner et al

Demineralization of bovine teeth (n = 60) in acid buffer

Preparation of standardized Class V cavities

Random assignment into 6 groups (n = 10 per group)


Infiltration and bonding procedure according to manufacturers’ instructions for use

Group 1 Group 2 Group 3 Group 4 Group 5 Group 6


Unfilled etch-and- Filled etch-and-rinse Self-etch adhesive Caries infiltrant Caries infiltrant Caries infiltrant
rinse adhesive adhesive (Icon) (Icon) (Icon)
iBond Self Etch
Syntac Classic Optibond FL Unfilled etch-and- Filled etch-and-rinse Self-etch
rinse adhesive adhesive adhesive
Syntac Classic Optibond FL iBond Self Etch

Enamel etching Enamel etching Enamel etching


Hydrochloric acid (120 s) Hydrochloric acid (120 s) Hydrochloric acid (120 s)
Icon-Dry (30 s) Icon-Dry (30 s) Icon-Dry (30 s)
Enamel infiltration (180 s) Enamel infiltration (180 s) Enamel infiltration (180 s)
Light curing (40 s) Light curing (40 s) Light curing (40 s)
Enamel infiltration (60 s) Enamel infiltration (60 s) Enamel infiltration (60 s)
Light curing (40 s) Light curing (40 s) Light curing (40 s)

Enamel and dentin etching Enamel and dentin etching iBond Self Etch (20 s) Dentin etching Dentin etching iBond Self Etch (20 s)
Phosphoric acid (15 s) Phosphoric acid (15 s) Light curing (20 s) Phosphoric acid (15 s) Phosphoric acid (15 s) Light curing (20 s)
Syntac Primer (15 s) Optibond FL Prime (15 s) Syntac Primer (15 s) Optibond FL Prime (15 s)
Syntac Adhesive (10 s) Optibond FL Adhesive Syntac Adhesive (10 s) Optibond FL Adhesive
Heliobond (15 s) (15 s) Heliobond (15 s) (15 s)
Light curing (20 s) Light curing (20 s) Light curing (20 s) Light curing (20 s)

Application of a nanofilled composite (Filtek Supreme XTE), light curing (20 s)

Thermocycling 5000x (5–55°C)

Replica production and quantitative margin analysis (scanning electron microscopy)

Statistical analysis

Fig 2 Experimental design.

Table 1 Composition of the caries infiltrant and adhesive systems used in the present study

Product Composition Lot number Manufacturer


Icon Icon-Etch: hydrochloric acid, pyrogenic silicic acid, surface-active substances 724868 DMG; Hamburg,
Icon-Dry: 99% ethanol 724860 Germany
Icon-Infiltrant: TEG-DMA-based resin matrix, initiators, additives 72854

Syntac Primer: dimethacrylates, maleic acid, solvent, stabilizer U43425 Ivoclar Vivadent;
Classic Adhesive: dimethacrylates, maleic acid, glutaraldehyde, water V01074 Schaan,
Heliobond: bis-GMA, TEG-DMA, stabilizers and catalysts T15984 Liechtenstein

Optibond Primer: HEMA, GPDM, ethanol, water, CQ, BHT, PAMA 5554307 Kerr; Orange, CA,
FL Adhesive: bis-GMA, HEMA, GDM, CQ, ODMAB, barium aluminumborosilicate, Na2SiF6, 5543327 USA
fumed silicon dioxide, gamma-methacryloxypropyltrimethoxysilane

iBond UDMA, 4-META, glutaraldehyde, acetone, water, photo-initiators, stabilizers 010901 Heraeus Kulzer;
Self Etch Hanau, Germany

4-META: 4-methacryloyloxethyl trimellitate anhydride; BHT: butylhydroxytoluene; bis-GMA: bisphenol-A-glycidyldimethacrylate; CQ: camphorquinone; GDM: glyc-
erol dimethacrylate; GPDM: glycerolphosphatedimethacrylate; HEMA: 2-hydroxylethyl methacrylate; ODMAB: 2-(ethylhexyl)-4-(dimethylamino)benzoate; PAMA:
phthailic acid monomethacrylate; TEG-DMA: triethylene glycol dimethacrylate; UDMA: urethane dimethacrylate.

Vol 19, No 6, 2017 485


Körner et al

B b A a C b
p = 0.039 p = 0.161 p < 0.001
100 Fig 3 Percentages of continuous
enamel margins of composite restor-
80 ations with and without infiltrant pre-
treatment before application of the
different adhesives. The boxplots show
60 the medians (black lines) with 25%
% and 75% quartiles (boxes); the whis-
40 kers represent 1.5*IQR (interquartile
range) or minima and maxima of the
distribution if below 1.5*IQR; outliers
20 are shown as circles. Statistically sig-
nificant differences (p < 0.05) in the
0 group 1 group 4 group 2 group 5 group 3 group 6 percentage of continuous margins be-
Syntac Classic Optibond FL iBond Self Etch tween different adhesives are marked
with different lower-case (within infil-
without infiltrant with infiltrant trant-pretreated groups) and capital let-
ters (within non-pretreated groups).

gel (Icon-Etch, DMG; Hamburg, Germany) for 120 s fol- Assessment of Margin Integrity
lowed by rinsing with water for 30 s. After drying the sur- After thermocycling, negative copies of each restoration
face with ethanol (Icon-Dry, DMG) for 30 s, the caries were taken with an A-polyvinylsiloxane material (President
infiltrant was applied to the pretreated surface for 180 s Light Body Coltène; Altstätten, Switzerland). To receive pos-
and light cured for 40 s. To complete the infiltration pro- itive replicas, the impressions were poured with epoxy resin
cedure, the infiltrant was re-applied for 60 s and light (Epoxyharz L, R&G Faserverbundwerkstoffe; Waldenbuch,
cured for another 40 s. Subsequently, the unfilled etch- Germany) before being glued to aluminum carriers (Ce-
and-rinse adhesive Syntac Classic was applied as de- mentit Universal, Merz&Benteli; Niederwangen, Switzer-
scribed in group 1. land). The replicas were sputter coated with gold (Sputter
y Group 5: Caries infiltrant + filled etch-and-rinse adhe- SCD 030, Balzers Union; Balzers, Liechtenstein) and sub-
sive (Optibond FL) jected to quantitative margin analysis using scanning elec-
The caries infiltrant was applied as described above. tron microscopy at 20 kV and 200X magnification (Vega
Subsequently, the filled etch-and-rinse adhesive Opti- TS5136XM, Tescan; Brno, Czech Republic). Margin quali-
bond FL was applied as described in group 2. ties were classified as “continuous”, “non-continuous” or
y Group 6: Caries infiltrant + self-etch adhesive (iBond “not judgeable” by one trained and blinded examiner
Self Etch) (M.G.), as performed in previous studies.5,16 The margin
The caries infiltrant was applied as described above. integrity between enamel and restoration was expressed in
Subsequently, the self-etch adhesive iBond Self Etch percentage of “continuous margin” in relation to the entire
was applied as described in group 3. assessable margin.11

Composite Application and Thermocycling Statistical Analysis


All pretreated Class V cavities were filled in one increment Descriptive statistics such as means and standard deviation
with a nanofilled composite material (Filtek Supreme XTE, were computed. The percentage of continuous margin was
3M ESPE; shade A2B, lot N535229), and light cured for arcsine transformed to achieve homogeneity of variance and
20 s. Excess was removed by using surgical scalpel blades normal distribution of residuals, and thus to accomplish the
(No. 12D, Gebr. Martin; Tuttlingen, Germany), and the fill- model assumption of ANOVA. A two-way ANOVA with the two
ings were finished and polished with silicon instruments factors “infiltrant pretreatment” (2 levels) and “adhesive” (3
(Brownie Mini-Points and Greenie Mini-Points, Shofu; San levels) including interaction was applied. Differences in the
Marcos, CA, USA) and polishing brushes (Occlubrush, Kerr). percentage of continuous margins between different adhe-
The restorations were checked using a microscope at 25X sives (within the infiltrant-pretreated and non-pretreated
magnification (Stemi 2000, Zeiss; Oberkochen, Germany). groups) were analyzed using one-way ANOVA and Tukey’s
Afterwards, the specimens were thermocycled 5000 times HSD post-hoc test. Two-sample t-tests were used to investi-
in water between 5°C and 55°C with a dwell time of 20 s in gate the influence of the infiltrant pretreatment within the
each temperature bath and a transfer time of 10 s (Willy- different adhesive groups. The level of significance was set
tec; Gräfelfing, Germany).49 at 5%. All statistical analyses and plots were performed
using R version 3.2.2 (The R Foundation for Statistical Com-
puting; Vienna, Austria; www.R-project.org).

486 The Journal of Adhesive Dentistry


Körner et al

400 μm 400 μm

Fig 4 SEM micrograph of continuous margin (group 5; Syntac Clas- Fig 5 SEM micrograph of discontinuous margin (group 3; iBond
sic with infiltrant pretreatment). Self Etch without infiltrant pretreatment).

RESULTS proposed as a suitable alternative to human enamel.34


Evaluation of margin integrity was performed by one trained
The percentage of continuous margins (margin integrity) and blinded examiner, as in previous studies.5,16 Neverthe-
after application of the three adhesives with and without less, the fact that only one examiner evaluated margin qual-
infiltrant pretreatment is given in Fig 3. Two-way ANOVA ity might be a shortcoming of the present study. Artificial
demonstrated statistical significance for the two factors enamel lesions were created, similar to previous in vitro
“adhesive” (p < 0.001) and “infiltrant pretreatment” studies investigating resin infiltration, and were proven to
(p < 0.001), as well as for their interaction (p = 0.001). have a histological structure comparable to white-spot le-
The significantly highest margin integrity was observed sions and enamel caries.25,27,30,38 It should be noted, how-
for Optibond FL, whether or not the demineralized enamel ever, that natural enamel lesions might be deeper than ar-
was pretreated with the infiltrant. While Syntac Classic tificial ones, possibly leading to different penetration of
showed better results in terms of margin integrity compared infiltrant and adhesives under natural conditions.41
to iBond Self Etch when no infiltrant was applied The type of etching, filler content, resin viscosity, and
(p = 0.009), the two adhesives showed similar results after penetration ability of adhesives are key factors for the de-
infiltrant pretreatment (p > 0.05). gree of margin integrity of adhesive restorations.44,45 To
Pretreatment of demineralized enamel with the infiltrant cover a broad spectrum of these characteristics, the three
resulted in a significant increase in margin integrity when different adhesives used in this study were chosen as com-
the unfilled etch-and-rinse adhesive Syntac Classic monly used, sound representatives of their respective
(p = 0.039) or the self-etch adhesive iBond Self Etch group. In order to create an adequate etching pattern and
(p < 0.001) was applied, but showed no significant improve- enable deep resin penetration, specimens were treated ac-
ment when the filled etch-and-rinse adhesive Optibond FL cording to manufacturers’ recommendations, which is in
(p = 0.161) was used. conformity with previous studies examining resin infiltration
SEM micrographs of continuous and non-continuous mar- on artificial lesions.3,19,50 Thus, etching was performed with
gins are illustrated in Figs 4 and 5. 15% hydrochloric acid before infiltrant application, with 37%
phosphoric acid before application of the etch-and-rinse ad-
hesives, and acidic self-etch monomers. Previous studies
DISCUSSION showed that the surface layer of enamel carious lesions
can be eroded almost completely by etching with
The present study demonstrated that pretreatment of de- hydrochloric acid, leading to better resin penetration into
mineralized enamel with caries infiltrant prior to adhesive the bulk of the carious lesion.3,33,37 The etching efficacy of
application improved the margin integrity of composite res- acidic monomers in self-etch adhesives is much lower com-
torations when either the unfilled or self-etch adhesive was pared to conventional acids, resulting in shallower demin-
used, but had no positive effect in combination with the eralization, a less regular etching pattern,15,30 and limited
filled adhesive. Thus, the first null hypothesis was partly resin penetration into the lesion bulk.9 The enamel margin
rejected. integrity of self-etch adhesives has been shown to benefit
In this study, margin integrity was evaluated on bovine from pre-etching with phosphoric acid.43,46 The results of
teeth, which are widely used in resin infiltration tests and the present study indicate that a positive effect on margin

Vol 19, No 6, 2017 487


Körner et al

quality can also be achieved through pre-etching enamel enamel, leading to shallower demineralization, a more ir-
with hydrochloric acid, in case a self-etch adhesive is com- regular etching pattern, and thus limited resin penetra-
bined with a caries infiltrant. tion.10,17,31
Besides adequate etching, resin penetration ability is
affected by the viscosity and filler content of the infiltrant/
adhesive.48 In previous studies, it has been shown that CONCLUSION
resin infiltrants containing high amounts of TEG-DMA and
ethanol can decrease the viscosity and contact angle to The use of a caries infiltrant in demineralized enamel prior
enamel, allowing a better penetration coefficient and to adhesive application can improve margin integrity of com-
deeper penetration into demineralized enamel compared to posite restorations bonded with the tested self-etch and
resins containing bis-GMA or UDMA.28,36 On the other unfilled adhesives.
hand, it has also been reported that an increased amount
of TEG-DMA may lead to higher polymerization shrinkage
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Vol 19, No 6, 2017 489


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